US20040194223A1 - Method and apparatus for treatment of textile materials - Google Patents

Method and apparatus for treatment of textile materials Download PDF

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Publication number
US20040194223A1
US20040194223A1 US10/477,027 US47702704A US2004194223A1 US 20040194223 A1 US20040194223 A1 US 20040194223A1 US 47702704 A US47702704 A US 47702704A US 2004194223 A1 US2004194223 A1 US 2004194223A1
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Prior art keywords
dielectric body
electrodes
situated
plasma
textile
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Abandoned
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US10/477,027
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English (en)
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Mirko Cernak
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Pegas Nonwovens sro
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Individual
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Assigned to PEGAS NONWOVENS S.R.O. reassignment PEGAS NONWOVENS S.R.O. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CERNAK, MIRKO
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32348—Dielectric barrier discharge
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • D06M10/025—Corona discharge or low temperature plasma
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50—Modified hand or grip properties; Softening compositions

Definitions

  • the invention relates to a method and apparatus for treatment of inner and outer surfaces of woven and non-woven textiles and cords from organic and inorganic fibers with the aim to change surface properties of the fibers such as, first of all, hydrophilicity, hydrophobicity, surface energy, adhesion to other materials, colorability, surface electrical conductivity, and biocompactibility.
  • Textiles are made from organic or inorganic fibers that often do not possess the surface properties needed for given applications such as, for example, hydrophilicity, hydrophobicity, surface energy, adhesion to other materials, dyeability, surface electrical conductivity, and biocompactibility.
  • the surface properties of fibers situated inside of the textile material or on the outer textile material surfaces can be modified by various chemical methods described in, for example, F. Baldwin: “The chemical finishing of nonwovens”, INDA-TEC 97, pp. 6.0-6.42, as well as in patent applications DE 19,647,458; WO 97/11989; JP 09241980; and JP 09158020.
  • the plasmachemical methods are based on the use of low temperature electrical plasmas.
  • the low temperature plasmas as described herein are partially ionized and consist of activated species including gas molecules, ions, electrons, free radicals, metastables, and photons in the short wave ultraviolet range. While the gas temperature is low, the electrons have energies of several electron volts, corresponding to the temperatures on the order of 10 4 K. The electrons in collisions with gas molecules generate excited gas species, which can react with a variety of substrates to achieve modifications of surface properties.
  • volume barrier discharge was generated by applying a high frequency, high voltage signal to an electrode separated from an earthen plane or cylinder by a discharge gap and a dielectric barrier.
  • the fabric treated is localized on the dielectric barrier surface between both electrodes.
  • the main drawback of such volume barrier discharge devices used for textile treatment is that the useful plasma conditions are achieved only in small volume plasma channels termed “streamers” developing perpendicularly to the textile fibers. As a consequence, the plasma is in a very limited contact with the textile fiber surfaces, which results in non-uniform treatment and long treatment times.
  • JP 10241827 and JP 10139947 disclose atmospheric-pressure plasma apparatus for the treatment of textiles and fibers energized by fast-rising high-voltage pulses, where the treated material is localized between the electrodes. Besides apparent safety and electromagnetic interference problems, such energization is technically and economically problematic.
  • Patent JP 100087857 An atmospheric-pressure plasmachemical method for the treatment of skin surface of textile materials is disclosed in patent JP 100087857.
  • the device described there differs from the volume barrier discharge devices chiefly in that the streamers are parallel with the fabric surface, and the discharge electrodes are situated on the same side of the treated textile material. In this way, using a surface barrier discharge, the plasma is in a better contact with the surface, which reduces the treatment time significantly.
  • the patent discloses the treatment of a thin skin layer of the textile only, and the described method does not effect the properties of the surfaces of the textile materials.
  • the use of an optimized apparatus with the same electrode arrangement as in patent JP 100087857 for the textile treatment including the inner textile surface treatment is described, for example, in M. Cernak et al.: Prof.
  • the electrode surface erosion and abrasion is eliminated in apparatus where the coplanar surface discharge is used.
  • the coplanar surface discharge is described, for example, in A. Sato et al.: IEEE Trans. Electron Devices 23 (1976) 328, M. Haacke and G. J. Pietch: Proc. of XII Int. Conf. on Gas Discharges and their Appl., Glasgow, Sept. 2000, p. 267, V. I. Gibalov, G. J. Pietsch: J. Phys. D: Appl. Phys. 33 (2000) 2618, and E. H. Choi at al.: Jpn. J. Appl. Phys. 38 (1999) 6073.
  • Patent JP 3190077 describes the apparatus for ozone production where besides the main electrodes embedded in the dielectric body an auxiliary electrode situated on the dielectric body surface is used to generate a coplanar surface discharge.
  • Such a surface auxiliary electrode has the disadvantage of its limited lifetime due to an interaction with the discharge plasma.
  • U.S. Pat. No. 5,407,639 describes the auxiliary electrode of a coplanar surface discharge electrode system, which is embedded in the dielectric body. The aim of such a electrode is to initiate the discharge at reduced voltage values and increase its power for ozone production.
  • the present invention relates to the use of the known coplanar surface discharge for treatment of inner and outer surfaces of woven and non-woven textiles and cords from organic and inorganic fibers.
  • the electrical plasma is produced by electrical discharges generated using a discharge electrode system that comprises at least two electrically conductive electrodes situated on the same side of the treated textile material inside of a dielectric body.
  • the electrodes are energized by electrical voltage at a frequency from 50 Hz to 1 MHz and magnitude from 100 V to 100 kV, and the electrical discharges take place in a working gas at a pressure ranging from 1 kPa to 1,000 kPa above a part of the dielectric body surface, wherein the plasma is generated without a contact with the conductive electrodes.
  • the conductive electrodes are situated in parallel with the part of the dielectric body surface above which the plasma is generated.
  • the part of the dielectric body surface above which the plasma is generated has the shape of a given pattern.
  • the apparatus comprises the electrode system consisting of at least two electrically conductive electrodes, which are situated inside of a dielectric body, and an auxiliary system of electrodes also situated inside of the dielectric body.
  • the electrode systems are situated on both sides of the treated textile material.
  • the part of the dielectric body surface above which the plasma is generated has the shape of a plane surface, curved surface, or cylindrical surface.
  • a part of the dielectric body inside of which the electrodes are situated is made from a ferroelectric or liquid dielectric material.
  • the electrode edges are curved.
  • a part of the dielectric body inside of which the electrodes are situated contains MgO.
  • the electrical plasma is generated by electrical discharges in the vicinity of the dielectric body surface, wherein a part of the dielectric body insulating the electrodes from each other as well as from the electrical plasma is made preferably from a ferroelectric material.
  • the treated textile material is situated on the part of the dielectric body surface above which the plasma is generated, or is in motion along the part of the dielectric body surface above which the plasma is generated, in a direct contact with this surface, or in close vicinity of this surface, in such a way that the discharge electrodes of the electrode system are embedded inside the dielectric body on the same side of the treated textile material.
  • Such an electrode arrangement is characterized by the fact that all or the majority of electrical field lines enter and go out from the treated textile on the same side of the treated textile and by the fact that the discharge electrodes are not in a contact with the electrical plasma.
  • the electric field lines and the electrical discharge channels have the direction mostly parallel with the textile fiber surfaces and the electrode lifetime is not reduced by oxidation or erosion due to a contact with the plasma, and due to the abrasion by the treated textile.
  • An alternating or pulsed electrical voltage of a magnitude ranging from 100 V to 100 kV and a frequency ranging from 50 Hz to 1 MHz is applied between the discharge electrodes serving to generate the discharge.
  • the apparatus can operate over a wide pressure range from on the order of 1 kPa to the order of 1,000 kPa, preferably at atmospheric gas pressure.
  • FIG. 1 is a schematic cross-sectional view illustrating a part of the planar electrode system for the surface discharge generation that can be an essential part of the apparatus schematically illustrated by FIG. 3 and FIG. 4.
  • FIG. 2 is a schematic cross-sectional view illustrating a part of the electrode system with a cylindrical surface shape, which is equipped with an auxiliary electrode structure and can be a substantial part of the apparatus illustrated in FIG. 5.
  • FIG. 3 is a side sectional view schematically illustrating the apparatus aimed to treat textile materials from one side, where the treated textile material is moved along the planar electrode system shown schematically in FIG. 1.
  • FIG. 4 is a side sectional view of the apparatus aimed to treat textile materials from both sides, where the treated textile material is moved between two electrode systems as that one illustrated schematically in FIG. 1.
  • FIG. 5 is a side sectional view of the device, where the treated textile material is brought into close contact with the cylindrical surface of the electrode system that is illustrated schematically in FIG. 2.
  • FIG. 1 In the device used for the surface treatment of textile materials from one side, which is illustrated by FIG. 1, the treated textile material 4 was moved continuously on the surface of the electrode system 1 .
  • the electrode system 1 is in detail illustrated in FIG. 1.
  • the textile material 4 was moved by means of two pairs of rolls 7 and 8 .
  • the space between both pairs of rollers was sealed by an upper wall 9 , bottom wall 10 , and by side walls that are not shown.
  • a working gas with a pressure a little above the atmospheric pressure was fed into the sealed space.
  • An electrical plasma was generated in the working gas on the surface of the electrode system 1 .
  • the electrode system 1 was situated on the surface of a cooler 11 .
  • the dielectric body 5 shown in FIG. 1 comprised a 0.5-mm-thick Al 2 O 3 layer with the coplanar metallic electrodes 2 and 3 deposited by vacuum sputtering and subsequent electroplating on its bottom surface and of a solid dielectric layer coating the Al 2 O 3 layer and electrodes 2 and 3 from their bottom side. An alternating electrical voltage was applied between the electrodes 2 and 3 . The frequency of the voltage was 25 kHz and the voltage was 10 kV peak-to-peak.
  • a non-woven polypropylene textile (spunbond, 15 g/m 2 , 2.8-3.2 dtex) was treated according to the invention.
  • the aim was to impart hydrophilicity to fiber surfaces in the whole volume of the textile and, consequently, to improve perviousness of the textile for water, urine, and other liquids.
  • the non-woven fabric was treated by the plasma generated in nitrogen using the device described in Example 1.
  • the strike-through time of test liquid through the textile was measured using a standard ETR 150.3-96 method.
  • the exposure time of 0.8 s resulted in a 30-fold reduction in the strike-through time.
  • the method according to the present invention was used for a hydrophilic treatment of biodegradable PLA textile of square weight of 15 g/m 2 .
  • the aim of the treatment was to impart hydrophilicity to fiber surfaces in the whole volume of the textile and, consequently, to improve perviousness of the textile for water, urine, and other liquids.
  • the textile was treated using the apparatus described in Example 1 in a CO 2 plasma.
  • the exposure time of 1.2 s resulted in the permanent strike-through time value of 3 s.
  • the method according to the present invention was used for hydrophilic treatment of a non-woven polypropylene textile (spunbond, 18 g/m 2 , 2.8-3.2 dtex).
  • the aim was to impart the hydrophilicity to a portion of the textile in the shape of a given pattern for the application in baby diapers manufacturing.
  • the portion of the surface of the dielectric body 5 under which the electrodes 2 and 3 were situated had the shape of a given pattern, and the textile movement was interrupted for a treatment time of two seconds.
  • the 2 s treatment resulted in a 30-fold reduction in the strike-through time on the treated textile portion, whereas the rest of the textile remained hydrophobic.
  • the method according to the present invention was used for surface activation of a woven textile material made from E-glass (210 g/m 2 , 0.18 mm. thick) for the use as a reinforcement in composite materials.
  • the textile was treated in a mixture of nitrogen and water vapor at 80° C.
  • a treatment time of five seconds resulted in a fivefold higher density of surface OH groups measured by the ESCA method.
  • the method according to the present invention was used for surface activation of a thin skin layer of a thick (200 g/m 2 ) PP meltblown non-woven textile with the aim to increase textile surface energy and its adhesive properties for the following lamination.
  • a 2 s exposition of the textile to the plasma generated in nitrogen with 3%-admixture of hydrogen resulted in an increase of the surface energy from 30 N/m for the untreated textile to 72 N/m for the plasma-treated textile, and the adhesive properties were improved significantly.
  • the treated textile 4 was moved intermittently on the surface of the planar electrode system 1 .
  • the textile was moved intermittently for the length of the electrode system 1 in a one movement cycle using two pairs of guide rolls 7 and 8 .
  • the space between both pairs of rollers was sealed by an upper wall 9 , bottom wall 10 , and by side walls that are not shown.
  • a working gas with a pressure a little above the atmospheric pressure was fed into the sealed space.
  • An electrical plasma was generated in the working gas on the surface of the electrode system 1 .
  • the dielectric body 5 shown in FIG. 1 comprised a 0.25-mm-thick Al 2 O 3 layer with the coplanar metallic electrodes 2 and 3 deposited by vacuum sputtering and subsequent electroplating on its bottom surface and a solid dielectric layer coating the Al 2 O 3 layer and electrodes 2 and 3 from their bottom side.
  • the electrode system 1 was situated on the surface of a cooler 11 .
  • An alternating electrical voltage was applied between the electrodes 2 and 3 .
  • the frequency of the voltage was 5 kHz and the voltage was 5 kV peak-to-peak. From a plan view in the direction perpendicular to the electrode system 1 surface, the electrodes 2 and 3 covered the electrode system surface portion corresponding to the shape of a given pattern, where a thin plasma layer was generated in the shape of the given pattern.
  • the device illustrated in FIG. 7 was used for the textile treatment by plasma from both sides of the treated textile.
  • the treated textile 4 was moved between two planar electrode systems 1 .
  • the electrode system 1 is in detail illustrated by FIG. 1.
  • the electrode systems 1 used were identical with the electrode system 1 described in Example 1.
  • the treated textile 4 was moved by means of two pairs of rolls 7 and 8 .
  • the space between both pairs of rollers was sealed by an upper wall 9 , bottom wall 10 , and by side walls that are not shown.
  • a working gas with a pressure a little above the atmospheric pressure was fed into the sealed space.
  • An electrical plasma was generated in the working gas on the surface of the electrode system 1 .
  • the electrode system 1 has the shape of a cylinder envelope.
  • the treaded textile 4 was fed into and out of the apparatus by means of two pairs of rolls 7 and 8 . Inside of the device, the treated textile 4 was brought on the surface of the electrode system 1 by means of a pair of internal guide rolls 12 .
  • the space between the pairs of rolls 7 and 8 was sealed by an upper wall 9 , bottom wall 10 , and by side walls that are not shown.
  • a working gas with a pressure a little above the atmospheric pressure was fed into the sealed space.
  • An electrical plasma was generated in the working gas on the surface of the electrode system 1 .
  • the glaze layer was deposited on the surface of a cooled ceramic cylinder and coplanar metallic electrodes 2 and 3 , having the shape of a system of 1-mm-wide parallel strips with the distance between the strips of 0.5 mm, were embedded in it.
  • the auxiliary electrode structure 11 was situated symmetrically between the electrodes 2 and 3 in such a way that the distance between the auxiliary electrode structure 11 surface and the surface of the electrode system 1 was 0.25 mm.
  • the auxiliary electrode structure 11 was made from 0.5-mm-diam. metallic wires.
  • the cylinder with the electrode system 1 on its surface rotated and carried the treated textile 4 on its surface.
  • the frequency of the voltage applied between the electrodes 2 and 3 was 5 kHz and the voltage was 12 kV peak-to-peak.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
US10/477,027 2001-05-04 2002-05-03 Method and apparatus for treatment of textile materials Abandoned US20040194223A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SK629-2001A SK6292001A3 (en) 2001-05-04 2001-05-04 Method and device for the treatment of textile materials
SKPV629-2001 2001-05-04
PCT/SK2002/000008 WO2002095115A1 (en) 2001-05-04 2002-05-03 Method and apparatus for treatments of textile materials

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US (1) US20040194223A1 (cs)
EP (1) EP1387901B1 (cs)
AT (1) ATE377109T1 (cs)
CZ (1) CZ300574B6 (cs)
DE (1) DE60223240T2 (cs)
DK (1) DK1387901T3 (cs)
ES (1) ES2296939T3 (cs)
SK (1) SK6292001A3 (cs)
WO (1) WO2002095115A1 (cs)

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EP1741826A1 (en) 2005-07-08 2007-01-10 Nederlandse Organisatie voor Toegepast-Natuuurwetenschappelijk Onderzoek TNO Method for depositing a polymer layer containing nanomaterial on a substrate material and apparatus
US20070148366A1 (en) * 2005-12-22 2007-06-28 Selwyn Gary S Side-specific treatment of textiles using plasmas
US20090194507A1 (en) * 2006-06-08 2009-08-06 Faculty Of Mathematics Physics And Informatics Comenius University Apparatus and method for cleaning, etching, activation and subsequent treatment of glass surfaces, glass surfaces coated by metal oxides, and surfaces of other si02-coated materials
US20090200948A1 (en) * 2008-02-11 2009-08-13 Apjet, Inc. Large area, atmospheric pressure plasma for downstream processing
US20100015358A1 (en) * 2006-12-05 2010-01-21 Faculty Of Mathematics, Physics And Informatics Of Commenius University Apparatus and method for surface finishing of metals and metalloids, metal oxides and metalloid oxides, and metal nitrides and metalloid nitrides
US20100163534A1 (en) * 2007-02-23 2010-07-01 Claudia Riccardi Atmospheric-plasma processing method for processing materials
US20100203257A1 (en) * 2007-01-10 2010-08-12 Nederlandse Oraganisatie Voor Toegepastnatuurwetenschappelijk Onderzoek Tno Method and Apparatus for Treating an Elongated Object with Plasma
US7999173B1 (en) 2007-03-21 2011-08-16 The United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration Dust removal from solar cells
US20110308457A1 (en) * 2008-12-30 2011-12-22 Nederlandse Organisatie Voor Toegepastnatuurwetens Chappelijk Onderzoek Tno Apparatus and method for treating an object
WO2012163876A1 (de) 2011-05-31 2012-12-06 Leibniz-Institut für Plasmaforschung und Technologie e.V. Vorrichtung und verfahren zur erzeugung eines kalten, homogenen plasmas unter atmosphärendruckbedingungen
WO2016138403A1 (en) * 2015-02-26 2016-09-01 Curt G. Joa, Inc. Apparatus and methods for modifying webs of material with plasma
WO2016193406A1 (de) 2015-06-04 2016-12-08 Hochschule Für Angewandte Wissenschaft Und Kunst Hildesheim/Holzminden/Göttingen Vorrichtung zur plasmabehandlung von insbesondere bandförmigen objekten
US10504703B2 (en) 2016-12-29 2019-12-10 Industrial Technology Research Institute Plasma treatment apparatus
US11041825B2 (en) * 2017-09-21 2021-06-22 Nanowear Inc. Methods, processes, and apparatus for depositing nanosensors on low surface energy substrates

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US20070117490A1 (en) * 2005-11-23 2007-05-24 Trillas Xavier C Process to produce nonwoven fabrics with totally or partially hydrophilic areas and hydrophobic areas
SK51092006A3 (sk) * 2006-12-05 2008-08-05 Fakulta Matematiky, Fyziky A Informatiky Univerzity Komensk�Ho Zariadenie a spôsob povrchovej úpravy dreva, drevených vlákien a materiálov na báze dreva
EP2488690B1 (en) * 2009-10-16 2014-05-21 Masarykova Univerzita Method for improving felting properties of animal fibres by plasma treatment
CZ305107B6 (cs) 2010-11-24 2015-05-06 Technická univerzita v Liberci Chromatografický substrát pro tenkovrstvou chromatografii nebo pro kolonovou chromatografii
DE102011010273A1 (de) 2011-02-02 2012-08-02 Cinogy Gmbh Verfahren zur Behandlung von menschlichem oder tierischem Haar und Gerät zur Durchführung des Verfahrens
CZ2011873A3 (cs) 2011-12-22 2013-07-03 Pegas Nonwovens S.R.O. Zarízení pro úpravu netkané textilie
CZ305675B6 (cs) * 2012-05-18 2016-02-03 Technická univerzita v Liberci Způsob zvýšení hydrostatické odolnosti vrstvy polymerních nanovláken, vrstva polymerních nanovláken se zvýšenou hydrostatickou odolností, a vícevrstvý textilní kompozit obsahující alespoň jednu takovou vrstvu
CZ309452B6 (cs) 2021-05-05 2023-01-25 Masarykova Univerzita Způsob spuštění samovolně se šířícího procesu redukce-exfoliace oxidu grafenu v porézním materiálu

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ES2296939T3 (es) 2008-05-01
DE60223240D1 (de) 2007-12-13
WO2002095115A1 (en) 2002-11-28
CZ300574B6 (cs) 2009-06-17
DK1387901T3 (da) 2008-03-10
DE60223240T2 (de) 2008-08-07
CZ20041180A3 (cs) 2005-03-16

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