EP0826431A1 - Procédé de production d'une peinture de réparation - Google Patents

Procédé de production d'une peinture de réparation Download PDF

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Publication number
EP0826431A1
EP0826431A1 EP97114719A EP97114719A EP0826431A1 EP 0826431 A1 EP0826431 A1 EP 0826431A1 EP 97114719 A EP97114719 A EP 97114719A EP 97114719 A EP97114719 A EP 97114719A EP 0826431 A1 EP0826431 A1 EP 0826431A1
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EP
European Patent Office
Prior art keywords
radiation
meth
pigmented
curing
binders
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.)
Granted
Application number
EP97114719A
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German (de)
English (en)
Other versions
EP0826431B1 (fr
Inventor
Wolfgang Dr. Diener
Peter Dr. Klostermann
Frank-Jürgen Krumpolt
Christine Kurz
Karin Dr. Maag
Hans-Ulrich Dr. Simmrock
Werner Dr. Lenhard
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.)
EIDP Inc
Original Assignee
Herberts GmbH
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Application filed by Herberts GmbH filed Critical Herberts GmbH
Publication of EP0826431A1 publication Critical patent/EP0826431A1/fr
Application granted granted Critical
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/005—Repairing damaged coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
    • B05D3/065—After-treatment
    • B05D3/067—Curing or cross-linking the coating

Definitions

  • the invention relates to a method for producing a multilayer Refinishing, which is used in particular in the field of Vehicle and vehicle parts painting.
  • the method is particularly suitable for Repair of body parts and smaller damaged areas.
  • a drying or hardening of the painted Vehicles or vehicle parts can either be at room temperature overnight or in less time due to forced drying or hardening, for example 30 minutes at 60 ° C in a cabin.
  • forced drying or hardening for example 30 minutes at 60 ° C in a cabin.
  • IR radiators are usually used to prevent drying force.
  • the procedure is, for example, that wet-wet on a basecoat after a short flash off, a clear coat is applied and both layers cured within 20-25 minutes using one or more IR emitters will. Especially for the refinishing of body parts and smaller ones Damage points exist for reasons of effectiveness, the necessary To further shorten drying or curing times.
  • DE-A-15 71 175 describes a method for curing an air-drying unsaturated polyester resin layer, which is in the wood coating Application. The curing takes place here with flashes of light from an electrical gas-filled flash tube.
  • DE-A-41 33 290 describes a method for producing a Multi-layer coating for automotive OEM painting described, in which a radiation-curable coating agent is used as the clear lacquer and the Application of the coating agent when illuminated with light of a wavelength of over 550 nm or in the absence of light and curing by means of high-energy radiation is carried out.
  • the clear coat is applied to a KTL primer, filler and basecoat coated and at 120-140 ° C baked substrate applied and then irradiated.
  • EP-A-0 000 407 describes a radiation-curable coating agent Basis of an OH-functional polyester resin esterified with acrylic acid, one Vinyl compound, a photoinitiator and a polyisocyanate.
  • a first Radiation curing takes place using UV light and in a second curing step
  • the hardening step gives the coating its final hardness through the OH / NCO crosslinking.
  • the second hardening step can take place at 130-200 ° C or over several days Room temperature.
  • the object of the invention was to provide a method for producing a multilayer Refinishing, in particular for refinishing vehicle parts and to repair smaller damaged areas, which the previously usual drying times reduced and coatings, which despite shortened Drying times without sacrificing quality meet the requirements of a Refinishing, especially regarding hardness, scratch resistance and elasticity are sufficient.
  • the object is achieved by a method for producing a multilayer Refinishing by applying an unpigmented or colorless pigmented transparent clear coat on a pre-dried or hardened color and / or effect basecoat or by applying a pigmented Topcoat layer on a possibly pre-coated substrate, which thereby is characterized in that for the production of the transparent clear coat or pigmented top coat only by radical and / or cationic Polymerization curable binders are used and the curing means pulsed high-energy UV radiation.
  • the one for hardening the transparent clear lacquer layer or the pigmented one Topcoat layer of high-energy pulsed UV radiation can be used for example generated with a radiation source, which is a High-energy electron flash device, hereinafter referred to as UV flash lamp, acts. With this radiation source, it is possible to cover the in the Fully harden within seconds.
  • a radiation source which is a High-energy electron flash device, hereinafter referred to as UV flash lamp
  • the multilayer structures obtained by the process according to the invention do the same for a property level required to show a refinishing, as under usual repair conditions dried or hardened multi-layer coatings.
  • a primer is applied if necessary and / or filler precoated substrate with a basecoat and wet-on-wet, if necessary after a short flash-off, a clear coat is applied. Then be both layers at room temperature overnight or within 20-80 min 40-80 ° C hardened.
  • the applied Basecoat is preferably only dried briefly and then the clearcoat is applied and subjected to radiation.
  • the clearcoat or pigmented topcoat is radiation-cured According to the invention with pulsed high-energy UV radiation.
  • a radiation source one or more UV flash lamps are preferably used for this purpose.
  • the UV flash lamps emit light with a wavelength of 200-900 nm Maximum at 500 nm.
  • the flashes can be triggered approximately every 4 s, for example will.
  • the UV flash lamps preferably contain a plurality of flash tubes, for example quartz tubes filled with inert gas such as xenon.
  • the UV flash lamps should have a on the surface of the coating to be hardened Illuminance of at least 10 megalux, preferably 10-80 megalux per Cause lightning discharge.
  • the electrical power per lightning discharge should be preferred 1-10 kJoules.
  • the UV flash lamp is preferably a Transportable device that is positioned directly in front of the damaged area to be repaired can be.
  • UV flash lamps that can be used are described, for example, in US Pat WO-A-9411123 and in EP-A-0-525 340.
  • UV flash lamps are commercially available.
  • the transparent clearcoats or pigmented top coats are radiation-curable coating agents that crosslink exclusively via radical and / or cationic polymerization.
  • These can be aqueous systems with high solids content, which are used as an emulsion are present, but the systems can also be in solvent-containing form. However, it is preferably 100% lacquer systems that do not contain solvents and can be applied without water.
  • All radiation-curable binders can be used in the process according to the invention customary radiation-curable binders or mixtures thereof are used, which are known to the person skilled in the art and are described in the literature. It is about either to be crosslinkable by radical polymerization or by cationic ones Polymerization crosslinkable binders. In the former arise through action from high-energy radiation to the binding agent or coating agent radicals that then trigger the crosslinking reaction. With the cationic curing systems are formed by irradiation from initiators Lewis acids, which then Trigger crosslinking reaction.
  • the free-radically curing binders can e.g. to prepolymers like Poly- or oligomers that contain olefinic double bonds in the molecule, act.
  • prepolymers or oligomers are (meth) acrylic functional (Meth) acrylic copolymers, epoxy resin (meth) acrylates, polyester (meth) acrylates, Polyether (meth) acrylates, polyurethane (meth) acrylates, unsaturated polyesters, Amino (meth) acrylates, melamine (meth) acrylates, unsaturated polyurethanes or Silicone (meth) acrylates.
  • the molecular weight (Mn) of these compounds is preferably from 200 to 10,000.
  • Aliphatic and / or cycloaliphatic (meth) acrylates used are particularly preferred (cyclo) aliphatic polyurethane (meth) acrylates and polyester (meth) acrylates.
  • the Binders can be used individually or in a mixture.
  • the prepolymers can optionally be used in so-called reactive diluents, i.e. reactive liquid monomers, dissolved.
  • the reactive thinners are in generally in amounts of 1-50 wt .-%, preferably 5-30 wt .-%, based on the Total weight of prepolymer and reactive thinner used.
  • the Reactive diluents can be mono-, di- or polyunsaturated. Examples for monounsaturated reactive diluents are: (meth) acrylic acid and its esters, Maleic acid and its half esters, vinyl acetate, vinyl ether, substituted Vinyl ureas, styrene, vinyl toluene.
  • unsaturated reactive thinners are: di (meth) acrylates such as alkylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, 1,3-butanediol di (meth) acrylate, vinyl (meth) acrylate, Allyl (meth) acrylate, divinylbenzene, dipropylene glycol di (meth) acrylate, hexanediol di (meth) acrylate.
  • di (meth) acrylates such as alkylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, 1,3-butanediol di (meth) acrylate, vinyl (meth) acrylate, Allyl (meth) acrylate, divinylbenzene, dipropylene glycol di (meth) acrylate, hexanediol di (meth) acrylate.
  • polyunsaturated reactive diluents are: glycerol tri (meth) acrylate, Trimethylolpropane tri (meth) acrylate, pentaerythritol tri (meth) acrylate, Pentaerythritol tetra (meth) acrylate.
  • the reactive diluents can be used individually or in Mixture can be used.
  • Preferred reactive thinners are diacrylates such as e.g. Dipropylene glycol diacrylate, tripropylene glycol diacrylate and / or Hexanediol diacrylate used.
  • the free-radically curable coating agents contain photoinitiators.
  • Suitable Photoinitiators are, for example, those in the wavelength range from 190 to Absorb 400 nm.
  • initiators for radical polymerization are chlorine-containing aromatic compounds, e.g. described in US-A-4 089 815, aromatic ketones as described in EP-A-0 003 002 and EP-A-0 161 463, Hydroxyalkylphenones as described in US-A-4,347,111.
  • Alkyl or arylphosphine oxides hydroxyacetophenone derivatives and Benzophenone derivatives.
  • the photoinitiators can, for example, in amounts of 0.1-5 wt .-%, preferably 0.5-3 wt .-%, based on the sum of radical polymerizable prepolymers, reactive diluents and initiators added will. They can be used individually or as mixtures.
  • Binders known to those skilled in the art and described in the literature are used will. These can be, for example, polyfunctional epoxy oligomers which contain more than two epoxy groups in the molecule. It is convenient if the binders are free from aromatic structures. Such epoxy oligomers are described for example in DE-A-36 15 790.
  • polyalkylene glycol diglycidyl ether hydrogenated bisphenol A glycidyl ether, Epoxy urethane resins, glycerol triglycidyl ether, diglycidyl hexahydrophthalate, Diglycidyl esters of dimer acids, epoxidized derivatives of (meth) cyclohexene, such as e.g. 3,4-epoxycyclohexylmethyl (3,4-epoxycyclohexane) carboxylate or epoxidized Polybutadiene.
  • the number average molecular weight of the polyepoxide compounds is preferably below 10,000.
  • Reactive diluents such as e.g. Cyclohexene oxide, butene oxide, butanediol diglycidyl ether or Hexanediol diglycidyl ether can be used.
  • Photoinitiators for cationic curing systems are substances that act as onium salts are known which photolytically release Lewis acids under the action of radiation. Examples include diazonium salts, sulfonium salts or iodonium salts. Triarylsulfonium salts are preferred.
  • the photonitiators can be used in quantities of 0.5 to 5 wt .-%, based on the sum of cationically polymerizable Prepolymers, reactive diluents and initiators, individually or as a mixture be used.
  • the transparent clearcoats and pigmented top coats can contain additives.
  • the additives are the usual additives that can be used in the paint sector.
  • Additives are leveling agents, e.g. based on (meth) acrylic homopolymers or silicone oils, rheology influencing agents, such as finely divided silica or polymeric urea compounds, thickeners, such as crosslinked polycarboxylic acid or Polyurethanes, anti-foaming agents, wetting and elasticizing agents.
  • leveling agents e.g. based on (meth) acrylic homopolymers or silicone oils
  • rheology influencing agents such as finely divided silica or polymeric urea compounds
  • thickeners such as crosslinked polycarboxylic acid or Polyurethanes
  • anti-foaming agents wetting and elasticizing agents.
  • light stabilizers are phenyl salicylates, Benzotriazole and derivatives, HALS compounds and oxalanilide derivatives.
  • the transparent clearcoats and pigmented top coats can contain organic solvents and / or water.
  • the solvents are common paint solvents. This can come from the manufacture of the binders or are sold separately admitted. Examples of such solvents are monohydric or polyhydric alcohols, e.g. Propanol, butanol, hexanol; Glycol ethers or esters, e.g. Diethylene glycol dialkyl ether, Dipropylene glycol dialkyl ether, each with C1 to C6 alkyl, Ethoxypropanol, butyl glycol; Glycols, e.g.
  • Ethylene glycol, propylene glycol and their oligomers N-methylpyrrolidone and ketones, e.g. Methyl ethyl ketone, acetone, Cyclohexanone; aromatic or aliphatic hydrocarbons, e.g. Toluene, xylene or linear or branched aliphatic C6-C12 hydrocarbons.
  • ketones e.g. Methyl ethyl ketone, acetone, Cyclohexanone
  • aromatic or aliphatic hydrocarbons e.g. Toluene, xylene or linear or branched aliphatic C6-C12 hydrocarbons.
  • the clear lacquers which can be used according to the invention can contain transparent pigments, such as e.g. Contain silicon dioxide, and possibly soluble dyes.
  • the invention usable pigmented topcoats contain color and / or effect Pigments.
  • pigments all common pigments are organic or suitable of inorganic nature. Examples of inorganic or organic Color pigments are titanium dioxide, micronized titanium dioxide, iron oxide pigments, carbon black, Azo pigments, phthalocyanine pigments, quinacridone and pyrrolopyrrole pigments. Examples of effect pigments are metal pigments, e.g. Aluminum pigments, and pearlescent pigments.
  • radical curing systems various cationic curing systems or radical and cationic curing systems can be combined. Radically curing systems are preferably used.
  • the radiation-curable coating agents can, in a known manner, for example, by spray application.
  • the transparent Clearcoats can be applied to conventional aqueous or solvent-based basecoats be applied.
  • Basecoats containing binders can be used.
  • the basecoats included organic and / or inorganic color and / or effect pigments and / or Fillers, water and / or organic solvents and, if necessary, additives common in paint.
  • the basecoats are applied to substrates that are coated with conventional primers, Filler and intermediate layers, such as those for multi-layer painting on the Motor vehicle sector can be used, can be pre-coated.
  • Preferred Substrates are metal or plastic parts.
  • the drying or hardening of the basecoat film can take place at room temperature or at elevated temperature. Drying can preferably take place within a few Minutes, e.g. 3-10 minutes, at 40-80 ° C. This is particularly preferably done Drying the basecoat using infrared radiation. The IR drying can for example within 3-6 minutes.
  • the clearcoat is applied, preferably in a resulting dry film layer thickness of 20-80 ⁇ m, preferred from 20-50 ⁇ m.
  • a pigmented topcoat is used as a radiation-curable coating agent, for example, this can be based on conventional solvent- or water-based fillers, Primers or intermediate layers can be applied. The pens-, Primer or intermediate layers can already be cured or be pre-dried.
  • the clearcoat is preferred in multi-layer refinishing radiation-curable coating agent formulated.
  • the Crosslinking using UV radiation After application of the clear coat or the pigmented top coat, the Crosslinking using UV radiation. They already serve as UV radiation sources described UV flash lamps.
  • the coatings can be dried or hardened by a plurality of successive lightning discharges. Prefers 1 to 40 successive lightning discharges are triggered.
  • the distance of the UV flash lamp to the substrate surface to be irradiated can be 5-50 cm, preferably 10-25 cm, particularly preferably 15-20 cm. Shielding the UV lamps to avoid radiation leakage can e.g. by Use an appropriately lined protective housing around the transportable Lamp unit or with the help of other, known to those skilled in the art Security measures.
  • the total irradiation time is in the range of a few seconds, for example in the range from 1 millisecond to 400 seconds, preferably from 4-160 seconds, each according to the number of selected lightning discharges.
  • the process according to the invention is particularly suitable for refinishing smaller body parts or smaller damaged areas, but can also be used Refinishing of larger parts, for example larger vehicle parts be used.
  • the pendulum damping test was carried out in accordance with DIN 53157 (according to König).
  • the Erichsen deepening was carried out according to ISO 1520.
  • a water-based lacquer (binder base: polyurethane resin) was applied to filler-coated KTL sheet in a resulting dry film layer thickness of 13-15 ⁇ m. It was dried for 3 minutes with an IR lamp. Subsequently, the clear coats according to system 1-6 were applied in a resulting dry film thickness of 40-50 ⁇ m.
  • UV curing was carried out using a UV flash lamp (3500 Ws) with 10 exposures (approx. 40 s) with an object distance of 20 cm.
  • the coating technology properties of the coatings thus obtained are as above shown in Tables 1 and 2.
  • the coatings are sufficient in terms of hardness, Scratch resistance and elasticity essentially meet the requirements of a Repair multi-coat paint can be provided.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)
  • Circuit Arrangement For Electric Light Sources In General (AREA)
  • Discharge Lamp (AREA)
  • Discharge-Lamp Control Circuits And Pulse- Feed Circuits (AREA)
EP97114719A 1996-08-31 1997-08-26 Utilisation d'une lampe eclaire pour la production d'une peinture de réparation Expired - Lifetime EP0826431B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19635447 1996-08-31
DE19635447A DE19635447C1 (de) 1996-08-31 1996-08-31 Verfahren zur Herstellung einer Reparaturlackierung

Publications (2)

Publication Number Publication Date
EP0826431A1 true EP0826431A1 (fr) 1998-03-04
EP0826431B1 EP0826431B1 (fr) 2003-04-23

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ID=7804328

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EP97114719A Expired - Lifetime EP0826431B1 (fr) 1996-08-31 1997-08-26 Utilisation d'une lampe eclaire pour la production d'une peinture de réparation

Country Status (10)

Country Link
US (1) US5932282A (fr)
EP (1) EP0826431B1 (fr)
JP (1) JPH1085660A (fr)
AT (1) ATE238107T1 (fr)
AU (1) AU3527897A (fr)
CA (1) CA2214281A1 (fr)
DE (2) DE19635447C1 (fr)
DK (1) DK0826431T3 (fr)
ES (1) ES2191795T3 (fr)
PT (1) PT826431E (fr)

Cited By (3)

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WO2011101269A1 (fr) 2010-02-19 2011-08-25 Momentive Performance Materials Gmbh Unité intégrale d'exposition à un rayonnement
WO2013024146A1 (fr) 2011-08-18 2013-02-21 Momentive Performance Materials Gmbh Unité de rayonnement et de moulage
WO2014200418A1 (fr) * 2013-06-13 2014-12-18 Caraway Ab C/O Nääs & Co Dispositif pour ou dans le traitement de surface d'objets

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ES2167953T3 (es) * 1997-11-20 2002-05-16 Du Pont Procedimiento para el laqueado de reparacion de capas multiples de substratos.
EP1032475A1 (fr) * 1997-11-20 2000-09-06 E.I. Dupont De Nemours And Company Procede de laquage multicouche de substrats
EP1032476B2 (fr) * 1997-11-20 2007-11-14 E.I. Du Pont De Nemours & Company Incorporated Procede de laquage multicouche de substrats
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WO2000032688A1 (fr) 1998-12-03 2000-06-08 The Dexter Corporation Compositions adhesives comprenant un agent retardateur
DE19927041A1 (de) * 1999-06-14 2000-12-21 Herberts Gmbh & Co Kg Verfahren zur Reparaturlackierung von Fehlstellen in Einbrennlackierungen mit Pulverlacken
US20040131347A1 (en) * 1999-09-28 2004-07-08 Robert Lowery Adaptive paint matching system and method
US6400906B1 (en) 1999-09-28 2002-06-04 Robert Lowery Adaptive paint matching system and method
ATE283117T1 (de) * 1999-10-02 2004-12-15 Du Pont Verfahren zur herstellung von basislack/klarlack- zweischichtlackierungen und/oder transparenten versiegelungsschichten
DE50111955D1 (de) * 2000-03-16 2007-03-15 Volkswagen Ag Verfahren zur kleinflächigen beseitigung von lackierungsfehlern
AU2002210574B2 (en) 2000-10-25 2006-08-24 Allnex Netherlands B.V. Photoactivatable water borne coating composition
US6432490B1 (en) 2001-02-12 2002-08-13 E. I. Du Pont De Nemours And Company Process for coating substrates
US20020132044A1 (en) * 2001-03-19 2002-09-19 Quarles James H. Scratch repair procedure
US6541078B2 (en) 2001-05-09 2003-04-01 E. I. Du Pont De Nemours And Company Process for coating substrates
US7361383B2 (en) * 2001-06-04 2008-04-22 E.I. Dupont De Nemours & Company Process for multilayer coating of substrates
US7399793B2 (en) * 2003-10-31 2008-07-15 Basf Corporation Coating composition curable with ultraviolet radiation
DE102005012588A1 (de) * 2005-03-18 2006-09-21 Basf Coatings Ag Integriertes Beschichtungsstoffsystem auf der Basis von mit UV-A-Strahlung härtbaren, lösemittelhaltigen Beschichtungsstoffen, Verfahren zu seiner Herstellung und seine Verwendung
DE102005012589B4 (de) * 2005-03-18 2007-06-14 Basf Coatings Ag Mit UV-A-Strahlung härtbares, lösemittelhaltiges Gemisch, Verfahren zu seiner Herstellung und seine Verwendung
JP2007292776A (ja) * 2007-06-01 2007-11-08 Denso Corp 表示板
EP2192447A1 (fr) 2008-11-27 2010-06-02 Akzo Nobel Coatings International B.V. Procédé d'application d'un motif sur un substrat
JP5622277B2 (ja) * 2010-08-25 2014-11-12 関西ペイント株式会社 複層塗膜形成方法及び塗装物品
HK1210740A1 (en) 2012-06-11 2016-05-06 迈图高新材料集团 Method for producing plastic compound molded bodies
US9862858B2 (en) * 2012-09-21 2018-01-09 Basf Coatings Gmbh Method for producing and repairing a multicoat color and/or effect paint system
US20230357470A1 (en) * 2022-05-05 2023-11-09 Illinois Tool Works Inc. Photocurable topcoat repair composition and method for the use thereof

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WO2011101269A1 (fr) 2010-02-19 2011-08-25 Momentive Performance Materials Gmbh Unité intégrale d'exposition à un rayonnement
DE102010002141A1 (de) 2010-02-19 2011-08-25 Momentive Performance Materials GmbH, 51373 Integrale Bestrahlungseinheit
WO2013024146A1 (fr) 2011-08-18 2013-02-21 Momentive Performance Materials Gmbh Unité de rayonnement et de moulage
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US9675997B2 (en) 2013-06-13 2017-06-13 Caraway Ab Device for, or in, the surface treatment of objects

Also Published As

Publication number Publication date
US5932282A (en) 1999-08-03
AU3527897A (en) 1998-03-05
ES2191795T3 (es) 2003-09-16
DK0826431T3 (da) 2003-07-28
ATE238107T1 (de) 2003-05-15
PT826431E (pt) 2003-09-30
JPH1085660A (ja) 1998-04-07
DE19635447C1 (de) 1997-11-20
EP0826431B1 (fr) 2003-04-23
CA2214281A1 (fr) 1998-02-28
DE59709894D1 (de) 2003-05-28

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