EP1089829A1 - Procede de laquage de carrosserie ou de parties de carrosserie de vehicule - Google Patents

Procede de laquage de carrosserie ou de parties de carrosserie de vehicule

Info

Publication number
EP1089829A1
EP1089829A1 EP00916938A EP00916938A EP1089829A1 EP 1089829 A1 EP1089829 A1 EP 1089829A1 EP 00916938 A EP00916938 A EP 00916938A EP 00916938 A EP00916938 A EP 00916938A EP 1089829 A1 EP1089829 A1 EP 1089829A1
Authority
EP
European Patent Office
Prior art keywords
radiation
layer
substrate
coating
curing
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
EP00916938A
Other languages
German (de)
English (en)
Other versions
EP1089829B1 (fr
Inventor
Karsten Blatter
Werner 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
EI Du Pont de Nemours and Co
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
Family has litigation
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Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Publication of EP1089829A1 publication Critical patent/EP1089829A1/fr
Application granted granted Critical
Publication of EP1089829B1 publication Critical patent/EP1089829B1/fr
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

Links

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
    • 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
    • B05D3/02—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 baking
    • B05D3/0254—After-treatment
    • B05D3/0263—After-treatment with IR heaters
    • 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
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/52—Two layers
    • B05D7/53—Base coat plus clear coat type

Definitions

  • the invention relates to a method for painting, in particular for multi-layer painting of vehicle bodies or their parts with in particular water-based paints, in particular in the field of vehicle refinishing.
  • Vehicle refinishing is increasingly replacing solvent-based paints with water-based paints.
  • the developed water-based paints have already reached a quality level that makes them equal to the solvent-based paints in a number of properties.
  • some properties have not yet reached the quality level of solvent-based paints.
  • water-thinnable basecoats, clearcoats and single-layer topcoats it is still problematic to ensure a uniform quality of the coating, in particular with regard to surface properties and interlayer adhesion under different external conditions. It is particularly difficult to reproducibly under ambient conditions with widely varying air humidity
  • the object of the invention was therefore to provide a process for multi-layer coating, in particular for vehicle refinishing, which makes it possible to use coatings with high and uniform quality of the coating, especially with regard to surface properties and interlayer adhesion, even when using water-based base, clear and single-layer top coats achieve.
  • the uniform quality of the coating should also be particularly important under widely varying environmental conditions
  • NIR radiation which is an object of the invention, for curing clearcoat layers or single-layer topcoat layers on vehicle bodies or parts thereof, in particular in the case of refinishing.
  • the NIR radiation (near infrared) used according to the invention is short-wave infrared radiation in the wavelength range from approximately 760 to approximately 1500 n; preferably 760 to 1200 nm.
  • Another object of the invention relates to a method for painting a
  • a one-coat topcoat coating agent is optionally subjected to a flash-off phase and the curing is then carried out by irradiation with NIR radiation in the wavelength range from 760 to 1500 nm.
  • Single-layer topcoat coatings can preferably be water-based. However, it is also possible to use solvent-based coating agents.
  • the method according to the invention can in particular be a method for multi-layer coating.
  • this may include
  • This top coat layer can for example consist of a color and / or effect solvent-based or water-based basecoat and a water-based clearcoat.
  • the top coat layer can also consist of a water-based pigmented single-layer top coat coating agent. For example, one can proceed in such a way that in the case of the application of the top coat layer
  • Topcoat coating agent in the form of a pigmented single-layer topcoat the topcoat layer is first optionally subjected to a flash-off phase and then cured by irradiation with NIR radiation and that in the case of application of the topcoat coating agent in the form of a basecoat / clearcoat structure, a basecoat film is first applied after the
  • Basecoat or wet-on-wet if appropriate after a flash-off phase, the clear coat is applied, optionally subjected to a flash-off phase and then cured by irradiation with NIR radiation.
  • NIR radiation in general for drying paints and varnishes is known.
  • the following fields of application are mentioned, for example: printing industry, film drying, pipe drying, wood coatings, powder coatings.
  • the particular advantages of NIR technology are the very rapid drying, especially with water-based paints, and the gentle drying through low heating of the substrate. None is known about possible applications of this technology in vehicle painting, in particular vehicle refinishing.
  • Single-layer topcoat layers can be solved in a multi-layer structure.
  • the irradiation with NIR radiation carried out in the method according to the invention can be carried out with a customary high-energy NIR radiator.
  • NIR emitters are commercially available (for example from Industrie
  • SerVis are, for example, high-performance halogen lamps with a radiation density of generally more than 1 W / cm 2 , preferably more than 10 W / cm 2 , for example up to 15 MW / m 2 .
  • the emitters for example, reach an emitter surface temperature (filament temperature) of over 2500 K, for example from 2500 to 3000 K.
  • Suitable emitters have, for example, an emission spectrum with a maximum between 750 and 1200 nm.
  • a flash-off phase is preferably switched on before the irradiation with NIR radiation.
  • the flash-off phase takes place in the usual way, for example in air or by blowing air, e.g. at temperatures from 10 to 80 ° C, in particular at room temperature.
  • the inflated air can also be warmed if necessary.
  • blow-off systems can be used, e.g.
  • the ventilation can be carried out by standing at room temperature.
  • Paint surface can be avoided.
  • Single-layer topcoat coating compositions are, for example, customary clearcoats and single-layer topcoats based on water, as known in the art, such as those in the field of
  • Vehicle painting, especially vehicle refinishing are used.
  • the clear lacquer and single-layer top coat coating compositions contain water-thinnable
  • the water-dilutable binders are the customary binders known to those skilled in the art for this purpose.
  • it can be a one-component or two-component water-dilutable binder system.
  • two-component binder systems are preferred.
  • one-component binder systems are those based on water-dilutable polyurethane, polyacrylate, polyester and / or alkyd resins.
  • the one-component binder systems can e.g. be physically or oxidatively drying.
  • water-dilutable two-component crosslinkable binder systems are those based on hydroxy-functional binders, such as, for example, polyurethane, polyester urethane and / or polyacrylate polyols, and polyisocyanates, on the basis of acetoacetyl-functional and (mem) aci7loyl-functional binders, and on the basis of (meth) acryloyl-functional binders or (meth) acryloyl and glycidyl functional ones Binders and polyamines.
  • hydroxy-functional binders such as, for example, polyurethane, polyester urethane and / or polyacrylate polyols, and polyisocyanates
  • acetoacetyl-functional and (mem) aci7loyl-functional binders and on the basis of (meth) acryloyl-functional binders or (meth) acryloyl and glycidyl functional ones Binders and
  • water-thinnable binders which are at least partially curable by means of high-energy radiation, preferably UV radiation.
  • the preferred free-radically curing binders can be prepolymers, such as poly- or oligers, which have free-radically polymerizable olefinic double bonds, in particular in the form of (meth) acryloyl groups in the molecule.
  • the prepolymers can be used in combination with reactive diluents, i.e. reactive liquid monomers.
  • prepolymers or oligomers are (meth) acryloyl-functional (meth) acrylic copolymers, epoxy resin (meth) acrylates, polyester (meth) acrylates, polyether (meth) acrylates, polyurethane (meth) acrylates, unsaturated polyesters, unsaturated polyurethanes or silicone (meth) acrylates with number average molecular masses (Mn) preferably in the range from 200 to 10,000, particularly preferably from 500 to 3000 and with an average of 2 to 20, preferably 3 to 10, radically polymerizable, olefinic double bonds per molecule.
  • Mn number average molecular masses
  • reactive diluents are used in amounts of 1 to 50% by weight, preferably 5 to 30% by weight, based on the total weight of prepolymers and reactive diluents. These are defined low-molecular compounds that can be mono-, di- or polyunsaturated. Examples of such reactive diluents are: (meth) acrylic acid and its esters, maleic acid and their
  • Half esters vinyl acetate, vinyl ether, substituted vinyl ureas, ethylene and propylene glycol di (meth) acrylate, 1,3- and 1,4-butanediol di (meth) acrylate, Vinyl (m ⁇ th) acrylate, allyl (meth) acrylate, glycerol tri, di and mono (meth) acrylate, trimethylolpropane tri, di and mono (meth) acrylate, styrene, vinyl toluene, divinylbenzene, pentaerythritol tri and - tetra (meth) acrylate, di- and tripropylene glycol di (meth) acrylate, hexanediol di (meth) acrylate, and mixtures thereof.
  • UV-curable binders are described for example in DE-A-41 33 290.
  • Basecoat coating compositions which can be used in the process according to the invention are, for example, customary basecoats known to the person skilled in the art, such as those in the area of
  • the basecoats can be water-based or solvent-based.
  • solvent-based basecoats are those based on polyacrylate and / or polyester resins, optionally in combination with melamine resins and cellulose esters.
  • waterborne basecoats are those based on physically drying polyurethane, polyurethane urea, polyester, polyester urethane and / or polyacrylate resins and their modifications, such as acrylated or silicon-modified polyurethane and / or polyester resins.
  • waterborne basecoats come from chemically crosslinking binder components, e.g. from binders containing hydroxyl groups and polyisocyanate crosslinkers.
  • water-thinnable binders which are at least partially curable by means of high-energy radiation, preferably UV radiation. These are preferably free-radically curable binders, as have already been mentioned above.
  • binder systems mentioned here for basecoats, clearcoats and single-layer topcoats are only an example of an enumeration.
  • the binder systems can be modified even further, and different crosslinking mechanisms can also be combined with one another, for example curing with UN radiation can be combined with a further crosslinking mechanism. Examples of the latter combination are described in the as yet unpublished German patent application by the same applicant P 198 187 35 and in WO-A-9800452 and DE-A-197 09 560.
  • Single-layer topcoat compositions contain coloring and / or effect pigments. All paint-typical pigments of organic or inorganic nature are suitable as color pigments. Examples of inorganic or organic color pigments are titanium dioxide, micronized titanium dioxide, iron oxide pigments, carbon black, azo pigments, phthalocyanine pigments, quinacridone or pyrrolopyrrole pigments.
  • effect pigments are metal pigments, e.g. made of aluminum, copper or other metals; Interference pigments, e.g. metal oxide coated metal pigments, e.g. titanium dioxide coated or mixed oxide coated aluminum, coated mica, e.g. titanium dioxide coated mica and graphite effect pigments.
  • Transparent pigments in particular can also be present in the clear lacquers that can be used.
  • the coating compositions which can be used in the process according to the invention can furthermore contain water and also organic solvents and additives customary in paint.
  • the organic solvents which may be present in the coating compositions are customary paint solvents. These can originate from the production of the binders or are added separately. In the case of water-based coating agents, they are preferably water-miscible solvents.
  • suitable solvents are monohydric or polyhydric alcohols, e.g. Propanol, butanol, hexanol; Glycol ethers or esters, e.g. Diethylene glycol dialkyl ether, Dipropylenglykoldialky lether, each with Cl to C6 alkyl, ethoxy propanol, 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.
  • the coating compositions can furthermore contain additives customary in paint.
  • additives customary in paint are leveling agents, rheology-influencing agents, such as highly disperse silica or polymeric urea compounds, thickeners, such as cross-linked polycarboxylic acid or polyurethanes, defoamers, wetting agents, anti-cratering agents, light stabilizers and hardening accelerators.
  • leveling agents such as highly disperse silica or polymeric urea compounds
  • thickeners such as cross-linked polycarboxylic acid or polyurethanes
  • defoamers such as cross-linked polycarboxylic acid or polyurethanes
  • wetting agents such as anti-cratering agents, light stabilizers and hardening accelerators.
  • the additives are used in customary amounts known to the person skilled in the art.
  • the topcoat coating compositions additionally contain photoinitiators, e.g. in amounts of 0.1 to 5% by weight, preferably 0.5 to 3% by weight, based on the sum of free-radically polymerizable prepolymers, reactive diluents and photoinitiators.
  • photoinitiators are benzoin and derivatives, acetophone and derivatives, e.g. 2,2- diactoxyacetophenone, benzophenone and derivatives, thioxanthone and derivatives, anthraquinone, 1-benzoylcyclohexanol, organophosphorus compounds, e.g. Acylphosphine oxides.
  • the photoinitiators can be used alone or in combination.
  • the binder components which are reactive with one another must be stored in a dry state and can only be mixed with one another shortly before application.
  • spray viscosity can be adjusted with water or organic solvents before application.
  • the application of the coating compositions in the process according to the invention can be carried out by customary methods, preferably by means of spray application.
  • the top layers are usually made from a coloring and / or effect-giving solvent- or water-based basecoat coating agent and a water-based clearcoat coating agent or from a water-based pigmented single-layer coating agent or additional coating agent or additional filler coating agent.
  • Substrates are metal and plastic substrates, in particular the substrates known in the automotive industry, such as iron, zinc, aluminum, magnesium, stainless steel or their alloys, as well as polyurethanes, polycarbonates or polyolefins.
  • a filler layer is usually first applied and cured to the optionally pretreated and / or precoated substrates.
  • the top coat layer can then be applied to the filler layer.
  • the basecoat is first applied.
  • the basecoat film can be cured at room temperature or forced at 40 to 80 ° C, for example.
  • the basecoat film can also be wet-on-wet, if necessary overcoated with the clearcoat after a flash-off phase, and then cured together with the clearcoat.
  • the basecoat film is dried using NIR radiation. The more precise procedure for NIR irradiation is explained below.
  • the clear lacquer is then applied.
  • a flash-off phase can follow in the preferred embodiment, e.g. within 5 to 45 minutes, preferably 15 to 40 minutes, e.g. 10 to 80 ° C, preferably at room temperature.
  • the radiation is carried out using NIR radiation. This irradiation can be carried out, for example, in a conveyor system equipped with an NIR emitter or with an NIR emitter positioned in front of the object to be irradiated or the location to be irradiated.
  • the first-mentioned possibility is offered for the refinishing of sensitive parts, whereby the speed of the strip and thus the duration of the irradiation can be varied.
  • belt speeds of 1.0 to 7.0 m / min can be set, which can correspond, for example, to radiation times of 2 to 20 s.
  • the distance between the NIR emitter and the object surface can be, for example, 10 to 60 cm.
  • the NIR radiator is positioned in front of the object to be irradiated or the point to be irradiated.
  • the irradiation time can be, for example, 1 to 300 s, and the object distance can be, for example, 5 to 60 cm.
  • object temperature temperatures can be set. For example, object temperatures of 80 to 150 ° C. can be set.
  • UV radiation sources with emissions in the wavelength range from 180 to 420 nm, in particular from 200 to 400 nm, are preferably used.
  • Corresponding UV radiation sources and UV technology belong to the prior art and are known to the person skilled in the art.
  • the single-layer topcoat is applied to the substrate, preferably to the filler layer.
  • a flash-off phase can preferably follow, as described above. After the flash-off phase, the
  • Irradiation with NIR radiation can be carried out, for example, in a conveyor system equipped with an NIR emitter or with an NIR emitter that is positioned in front of the object to be irradiated or the position to be irradiated.
  • a UV radiation as already described above, must also be connected.
  • An advantageous embodiment of the method according to the invention consists in also curing the applied filler layer with NIR radiation. It is possible, after application of, for example, an aqueous filler coating agent, to first subject the filler layer to drying by irradiation with NIR radiation after an optionally allowed venting phase.
  • the final hardening can then be carried out using a suitable hardening method.
  • the final curing can be carried out, for example, at room temperature, forced at higher temperatures, by irradiation with UV or IR or NIR radiation.
  • Final curing is preferably carried out using UV or NIR radiation.
  • the method according to the invention is preferably used in vehicle and vehicle parts painting, in particular in vehicle refinishing. However, it is also possible to use the method according to the invention in vehicle body painting, in particular in the case of refinishing in vehicle body painting.
  • topcoat layers with a uniform, reproducible quality with regard to interlayer adhesion and surface properties are achieved even under varying external conditions, in particular with greatly varying atmospheric humidity. Likewise, a uniform quality of the coating is also guaranteed at critical points such as sikken or edges.
  • the topcoat layers have very good hardness and scratch resistance. They can be polished very well after a short time.
  • the extremely short drying or curing time which is achieved with the method according to the invention, is also advantageous. This extremely short drying or hardening time is also not significantly impaired by the flash-off phase to be granted, if any, which also occurs in a conventional painting process with hardening, for example in an oven. Di ⁇
  • a water-based lacquer (originally manufactured in accordance with DE-A-196 43 802, manufacturing example 4) was applied in 15 layers of dry film. After a flash-off phase of 25 minutes at room temperature, a water-clear lacquer based on an OH-functional polyurethane resin and a polyisocyanate crosslinker (produced in accordance with WO-A-94/03511, Example 11) was applied in a resulting dry film layer thickness of 50 ⁇ m. After a flash-off phase of 35
  • Irradiation was carried out for minutes at room temperature using a NIR emitter (500 W / cm 2 ). The distance between the beam and the object was 10 cm and the irradiation time was 6 s.
  • a water-based paint (correspondingly DE-A-196 43 802, manufacturing example 4) was applied in a resulting dry film layer thickness of 13 to 15 ⁇ m. After a flash-off time of 10 minutes, irradiation is carried out using a NIR radiator (500 W / cm 2 ). The distance
  • Emitter / object was 10 cm, the irradiation time 6 s.
  • a clear water-based lacquer based on an OH-functional polyurethane resin and a polyisocyanate crosslinker (produced in accordance with WO-A-94/03511, Example 11) was then applied in a resulting dry film layer thickness of 50 ⁇ m. After a flash-off phase of 35 minutes at room temperature, the irradiation was carried out with a
  • NIR emitter 500 W / cm 2 .
  • the emitter / object distance was 10 cm, the irradiation time 6 s. Comparative example
  • the mudguards painted according to Examples 1 and 2 show a uniform, uniform optical surface quality with regard to fullness, gloss and gradient over the entire object, while according to Comparative Example 3 these properties are formed on the beads and edges unsatisfactorily.

Landscapes

  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

La présente invention concerne un procédé de laquage d'un substrat par application d'un produit de revêtement de laque transparente sur un substrat prérevêtu ou d'un produit de revêtement de couche unique de finition sur un substrat éventuellement prérevêtu, puis par durcissement, le substrat consistant en une carrosserie ou une partie de carrosserie de véhicule. Après l'application du produit de revêtement de laque transparente ou du produit de revêtement de couche unique de finition, le substrat est éventuellement soumis à une phase d'évacuation d'air, puis le durcissement est réalisé par exposition à des rayonnements dans la plage du proche infrarouge (longueur d'onde comprise entre 760 et 1500 nm).
EP00916938A 1999-03-25 2000-03-14 Procede de laquage de carrosserie ou de parties de carrosserie de vehicule Revoked EP1089829B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19913442 1999-03-25
DE19913442A DE19913442C2 (de) 1999-03-25 1999-03-25 Verfahren zur Lackierung von Fahrzeugkarossen oder deren Teilen
PCT/EP2000/002232 WO2000058027A1 (fr) 1999-03-25 2000-03-14 Procede de laquage de carrosserie ou de parties de carrosserie de vehicule

Publications (2)

Publication Number Publication Date
EP1089829A1 true EP1089829A1 (fr) 2001-04-11
EP1089829B1 EP1089829B1 (fr) 2005-01-05

Family

ID=7902302

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00916938A Revoked EP1089829B1 (fr) 1999-03-25 2000-03-14 Procede de laquage de carrosserie ou de parties de carrosserie de vehicule

Country Status (5)

Country Link
US (1) US6506458B1 (fr)
EP (1) EP1089829B1 (fr)
AT (1) ATE286435T1 (fr)
DE (2) DE19913442C2 (fr)
WO (1) WO2000058027A1 (fr)

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DE19857045C2 (de) * 1998-12-10 2001-02-01 Industrieservis Ges Fuer Innov Beschichtung von Gegenständen
US6280800B1 (en) * 2000-01-18 2001-08-28 E. I. Du Pont De Nemours And Company Process for coating metallic substrate surfaces
DE10009822C1 (de) * 2000-03-01 2001-12-06 Basf Coatings Ag Verfahren zur Herstellung von Beschichtungen, Klebschichten oder Dichtungen für grundierte oder ungrundierte Substrate und Substrate
AU2001293853A1 (en) * 2000-09-29 2002-04-08 Advanced Photonics Technologies Ag Method and arrangement for producing a coated thermosensitive article or container with thermosensitive contents
DE10048361C1 (de) * 2000-09-29 2002-06-06 Advanced Photonics Tech Ag Verfahren zur Herstellung eines beschichteten wärmeempfindlichen Artikels oder Behälters mit wärmeempfindlichem Inhalt
ATE285851T1 (de) * 2000-10-24 2005-01-15 Sidmar Nv Verfahren zur herstellung von lackierten metallblechen
US6432490B1 (en) 2001-02-12 2002-08-13 E. I. Du Pont De Nemours And Company Process for coating substrates
DE10106890B4 (de) * 2001-02-14 2006-10-05 Advanced Photonics Technologies Ag Verfahren und Anordnung zur Herstellung eines quasi-endlosen beschichteten, wickelfähigen Bleches
US6541078B2 (en) 2001-05-09 2003-04-01 E. I. Du Pont De Nemours And Company Process for coating substrates
DE10127962B4 (de) * 2001-06-08 2006-01-26 Audi Ag Trocknungsverfahren für auf Bauteile, insbesondere auf Fahrzeugkarosserien oder deren Teile applizierte Lackmaterialien und Vorrichtung zur Durchführung des Trocknungsverfahrens
US6701601B2 (en) * 2001-07-03 2004-03-09 Daimlerchrysler Corporation Metal body painting system and method
WO2003061850A1 (fr) 2002-01-21 2003-07-31 Kansai Paint Co., Ltd. Procede pour former un film de revetement
US7523484B2 (en) 2003-09-24 2009-04-21 Infoexpress, Inc. Systems and methods of controlling network access
DE102004016093A1 (de) * 2004-04-01 2005-10-20 Volkswagen Ag Verfahren zur Trocknung wenigstens einer Lackschicht auf einem Substrat
TW200734384A (en) * 2006-03-03 2007-09-16 Jie-Nan Lin Method for manufacturing scratch-resistant plastic surface and the structure
US20100183820A1 (en) * 2009-01-16 2010-07-22 Ford Global Technologies, Llc Methods for curing uv-curable coatings
JP6584103B2 (ja) * 2015-03-18 2019-10-02 キヤノン株式会社 撮像装置

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Also Published As

Publication number Publication date
EP1089829B1 (fr) 2005-01-05
ATE286435T1 (de) 2005-01-15
DE50009153D1 (de) 2005-02-10
DE19913442A1 (de) 2000-09-28
WO2000058027A1 (fr) 2000-10-05
US6506458B1 (en) 2003-01-14
DE19913442C2 (de) 2002-10-31

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