EP1449186B1 - Film de transfert par laser pour etiquetage durable d'elements constitutifs - Google Patents

Film de transfert par laser pour etiquetage durable d'elements constitutifs Download PDF

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Publication number
EP1449186B1
EP1449186B1 EP02781201A EP02781201A EP1449186B1 EP 1449186 B1 EP1449186 B1 EP 1449186B1 EP 02781201 A EP02781201 A EP 02781201A EP 02781201 A EP02781201 A EP 02781201A EP 1449186 B1 EP1449186 B1 EP 1449186B1
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EP
European Patent Office
Prior art keywords
layer
laser
transfer film
adhesive
film according
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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.)
Expired - Lifetime
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EP02781201A
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German (de)
English (en)
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EP1449186A2 (fr
Inventor
Sven Reiter
Arne Koops
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Tesa SE
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Tesa SE
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0041—Digital printing on surfaces other than ordinary paper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0041—Digital printing on surfaces other than ordinary paper
    • B41M5/007—Digital printing on surfaces other than ordinary paper on glass, ceramic, tiles, concrete, stones, etc.
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/0041—Digital printing on surfaces other than ordinary paper
    • B41M5/0052—Digital printing on surfaces other than ordinary paper by thermal printing

Definitions

  • the invention relates to a laser transfer film for permanently inscribing components from a carrier layer, wherein an adhesive layer with pigmented boundary layer is present on the lower side of the carrier layer.
  • the marking by means of laser labels and printed or painted metal signs is becoming increasingly important, especially in the automotive industry, especially for high-quality markings.
  • information and instructions such as tire pressure or fuel type for the future user on a variety of components of the car are placed.
  • important production data can be transported via a laser label.
  • the label can be labeled with a barcode.
  • an assembly team With a suitable reader, an assembly team has the opportunity to read information about the model, color and special features from the barcode directly on the production line.
  • sensitive safety data such as chassis and identification numbers are also placed on the vehicle by means of labels. In the event of theft or accident, this information is of great importance for tracing the vehicle and manufacturing stages.
  • the label material used must therefore counteract manipulation attempts, as far as possible forgery-proof. It must not be detached from the bonding surface in a non-destructive way. Additional safety is achieved through the high brittleness of the material in combination with high bond strengths.
  • the adhesive force of the material on the primer plays a major role. It is decisive for the resistance to a manipulation attempt by detachment.
  • labels can be completely separated from the substrate.
  • plastic substrates such as polyethylene or polypropylene shows the bond between adhesive and substrate weaknesses.
  • a special blade tool can be placed under the label at a shallow angle. By careful cutting movements, it is possible to raise an edge, creating a so-called grip. On this catfish one creates a point of attack, which simplifies a detachment.
  • the labels are not applied to the component with a laser label, but by means of an imprint, it is easy for third parties to wash off or scrub the label. Also, often simply rubbing the labeled object on a second article, for example, a package to weaken the individual letters or numbers
  • the US 5,914,165 A1 describes a multilayer composite consisting of an upper layer (second layer 12), an intermediate carrier layer (first layer 11) and an adhesive layer (14) applied to the lower side of the intermediate carrier layer.
  • the upper layer (second layer 12) may contain laser-sensitive pigments.
  • the EP 0 845 767 A1 describes a label with a carrier layer, preferably a carrier film, on the underside of an adhesive is applied.
  • a marking substance is homogeneously distributed. The marking substance is able to migrate through the layer of adhesive and to penetrate into the substrate on which the label is applied.
  • the object of the invention is to provide a laser transfer film which enables the rapid and precise labeling of arbitrary components, which meets the stated requirement of improved security against counterfeiting, which is not destructively detachable even with the aid of a cutting tool, while continuing in particular high contrast, high resolution, high temperature resistance and easy to use has.
  • the invention relates to a laser transfer film for permanent marking of components of at least one carrier layer, wherein on the lower side of the carrier layer, an adhesive layer is present over the entire surface, wherein the carrier layer and the adhesive layer are transparent or translucent and do not absorb a laser beam, characterized that on the lower side of the adhesive layer is applied over its entire surface a pigment layer which contains at least one laser-sensitive pigment which absorbs and sublimates the energy of a laser beam.
  • the backbone of the layer containing the laser-sensitive pigments also consists of the adhesive of the adhesive layer, so that the first adhesive layer and the pigment layer form a single homogeneous layer. Only in the edge region of the homogeneous layer, specifically on the side facing away from the carrier layer, are the pigments distributed in a particularly narrow region of the homogeneous layer, thus forming a kind of boundary layer.
  • a second adhesive layer is preferably applied to the pigment layer containing the laser-sensitive pigment.
  • the second adhesive layer may be applied in the form of dots or by screen printing, optionally also as edge printing, so that the transfer film can be bonded to the substrate in any desired manner.
  • the thicknesses of the individual layers are selected from the following ranges: Carrier layer (preferably PET) 12 ⁇ m to 240 ⁇ m, especially 25 ⁇ m to 100 ⁇ m Adhesive (preferably acrylate) 5 ⁇ m to 45 ⁇ m, especially 10 ⁇ m to 25 ⁇ m pigment layer 1 ⁇ m to 10 ⁇ m, especially 2 ⁇ m to 5 ⁇ m
  • the films which are to be used according to the invention must be transparent and / or translucent; at least they must be designed in such a way that absorption of the laser beam, which would lead to their destruction, is precluded. In particular, it is desirable if the support material does not absorb light within the wavelength range of 530 to 1064 nm.
  • support material can be preferably used films which are transparent in a further excellently designed variant of the invention, in particular monoaxially and biaxially stretched films based on polyolefins, then films based on stretched polyethylene or stretched copolymers containing Ethylene and / or polypropylene units, optionally also PVC films, films based on vinyl polymers, polyamides, polyesters, polyacetals, polycarbonates.
  • PET films are outstandingly suitable as a carrier.
  • films based on stretched polyethylene or stretched copolymers containing ethylene and / or polypropylene units can be used according to the invention as a carrier film.
  • Monoaxially stretched polypropylene is characterized by its very high tensile strength and low elongation in the longitudinal direction.
  • Preferred for the production of labels according to the invention are monoaxially stretched films based on polypropylene.
  • the laser transfer films according to the invention are single-layer, biaxially or monoaxially stretched films and multilayered, biaxial or monoaxial films based on polypropylene, which have a sufficiently strong bond between the layers, since delamination of the layers during use is disadvantageous.
  • Films based on rigid PVC are used for the production of laser transfer films as well as films based on soft PVC.
  • films based on rigid PVC are preferably used.
  • Polyester-based films for example polyethylene terephthalate, are likewise known and can likewise be used for the production of the transfer films according to the invention.
  • the former are prepared from only a single monomer by, for example, polycondensation of an ⁇ -hydroxycarboxylic acid 1 or by ring-opening polymerization of cyclic esters (lactones) 2, for example
  • the latter is synthesized by polycondensation of two complementary monomers, for example a diol 3 and a dicarboxylic acid 4:
  • polyesters are obtained in the polycondensation of trihydric or polyhydric alcohols with polyfunctional carboxylic acids.
  • the polyesters are generally also the polycarbonates (carbonic acid polyester) counted.
  • PET polyethylene terephthalate
  • PBT polybutylene terephthalate
  • PCDT poly (1,4-cyclohexanedimethylene terephthalate) s
  • the laser transfer films of the invention may contain a self-adhesive based on natural rubber, PUR, acrylates or styrene-isoprene-styrene block copolymers.
  • the self-adhesive composition used is in particular a commercially available pressure-sensitive adhesive based on PUR, acrylate or rubber.
  • an acrylate hotmelt base which has a K value of at least 20, in particular greater than 30, obtainable by concentrating a solution of such a composition into a system which can be processed as a hotmelt.
  • the concentration can take place in suitably equipped boilers or extruders, in particular in the concomitant degassing a vented extruder is preferred.
  • the solution of the composition may contain from 5 to 80% by weight, in particular from 30 to 70% by weight, of solvent.
  • solvents are preferably used, in particular low-boiling hydrocarbons, ketones, alcohols and / or esters.
  • single-screw, twin-screw or multi-screw extruders with one or in particular two or more degassing units are used.
  • benzoin derivatives may be copolymerized, such as benzoin acrylate or benzoin methacrylate, acrylic acid or methacrylic acid ester.
  • benzoin derivatives are in the EP 0 578 151 A1 described.
  • the adhesive on Acrylathotmelt-based can also be chemically crosslinked.
  • self-adhesive compositions of (meth) acrylic acid and esters thereof having 1 to 25 carbon atoms, maleic, fumaric and / or itaconic acid and / or their esters, substituted (meth) acrylamides, maleic anhydride and other vinyl compounds , used as vinyl esters, in particular vinyl acetate, vinyl alcohols and / or vinyl ethers.
  • the residual solvent content should be below 1% by weight.
  • An adhesive which is particularly suitable is a low molecular weight acrylate hot melt pressure-sensitive adhesive, such as that marketed under the name acResin UV or Acronal®, in particular Acronal DS 3458, by BASF.
  • This adhesive with a low K value obtains its application-oriented properties through a final radiation-induced crosslinking.
  • an adhesive which consists of the group of natural rubbers or synthetic rubbers or of any blend of natural rubbers and / or synthetic rubbers, wherein the natural rubber or natural rubbers in principle from all available qualities such as crepe, RSS, ADS , TSR or CV types, depending on the required level of purity and viscosity, and the synthetic rubber or the synthetic rubbers from the group of random copolymerized styrene-butadiene rubbers (SBR), butadiene rubbers (BR), the synthetic polyisoprenes ( IR), butyl rubbers (IIR), halogenated butyl rubbers (XIIR), acrylate rubbers (ACM), ethylene-vinyl acetate copolymers (EVA) and polyurethanes and / or blends thereof.
  • SBR random copolymerized styrene-butadiene rubbers
  • BR butadiene rubbers
  • IR butyl rubbers
  • XIIR halogenated butyl rubbers
  • thermoplastic elastomers having a weight proportion of 10 to 50% by weight, based on the total elastomer content.
  • SIS styrene-isoprene-styrene
  • SBS styrene-butadiene-styrene
  • tackifying resins all previously known adhesive resins described in the literature can be used without exception. Mention may be made representative of the rosins, their disproportionated, hydrogenated, polymerized, esterified derivatives and salts, the aliphatic and aromatic hydrocarbon resins, terpene resins and terpene phenolic resins. Any combination of these and other resins can be used to adjust the properties of the resulting adhesive as desired. On the presentation of the knowledge in the " Handbook of Pressure Sensitive Adhesive Technology "by Donatas Satas (van Nostrand, 1989 ) is explicitly pointed out.
  • Hydrocarbon resin is a collective term for thermoplastic, colorless to intense brown colored polymers having a molecular weight of generally ⁇ 2000.
  • coal tar resins In petroleum, coal tar and terpene resins.
  • the most important coal tar resins are the coumarone-indene resins.
  • the hydrocarbon resins are obtained by polymerization of the unsaturated compounds which can be isolated from the raw materials.
  • hydrocarbon resins are also calculated by polymerization of monomers such as styrene or by polycondensation (certain formaldehyde resins) accessible polymers having a correspondingly low molecular weight.
  • Hydrocarbon resins are products with a softening range varying from ⁇ 0 ° C (at 20 ° C liquid hydrocarbon resins) to> 200 ° C in a wide range and a density of about 0.9 to 1.2 g / cm 3 .
  • Rosin resin is understood to mean a natural resin derived from the crude resin of conifers. A distinction is made between three types of rosin: balsam resin as distillation residue of turpentine oil, root resin as extract of coniferous rootstocks and tall resin, the distillation residue of tall oil. The most important in terms of quantity is balsam resin.
  • Rosin is a brittle, transparent product of red to brown color. It is insoluble in water but soluble in many organic solvents such as (chlorinated) aliphatic and aromatic hydrocarbons, esters, ethers and ketones as well as in vegetable and mineral oils.
  • organic solvents such as (chlorinated) aliphatic and aromatic hydrocarbons, esters, ethers and ketones as well as in vegetable and mineral oils.
  • the softening point of rosin is in the range of about 70 to 80 ° C.
  • Rosin is a mixture of about 90% resin acids and 10% neutral substances (fatty acid esters, terpene alcohols and hydrocarbons).
  • the most important rosin resin acids are unsaturated carboxylic acids of the general formula C20H3002, abietic, neoabietic, levopimaric, pimaric, isopimaric, and palustric acids, in addition to hydrogenated and dehydrated abietic acid.
  • softener it is possible to use all known softening substances. These include, among others, the paraffinic and naphthenic oils, (functionalized) oligomers such as oligobutadienes, isoprenes, liquid nitrile rubbers, liquid terpene resins, vegetable and animal oils and fats, phthalates, functionalized acrylates.
  • paraffinic and naphthenic oils such as oligobutadienes, isoprenes, liquid nitrile rubbers, liquid terpene resins, vegetable and animal oils and fats, phthalates, functionalized acrylates.
  • thermally activatable chemical crosslinkers such as accelerated sulfur or sulfur donor systems, isocyanate systems, reactive melamine, formaldehyde and (optionally halogenated) phenol-formaldehyde resins or reactive phenolic resin or diisocyanate crosslinking systems with the corresponding activators, are epoxidized polyesters - And acrylate resins and their combinations used.
  • the crosslinkers are preferably activated at temperatures above 50 ° C, in particular at temperatures of 100 ° C to 160 ° C, most preferably at temperatures of 110 ° C to 140 ° C.
  • the thermal excitation of the crosslinker can also be effected by IR radiation or high-energy alternating fields.
  • the adhesives which are to be used according to the invention are transparent or translucent, they are designed in such a way that absorption of the laser beam, which would lead to their destruction, is precluded. In particular, it is desirable if the adhesive does not absorb light within the wavelength range of 530 to 1064 nm.
  • the laser-sensitive pigment is preferably applied to the first adhesive layer in the form of a solvent suspension, for example an isopropanol suspension.
  • the first adhesive view on the surface is in particular dissolved, so that the pigment can be deposited in the edge region of the adhesive layer, namely the boundary layer, by swelling of the adhesive polymer matrix, while Evaporates solvent.
  • the boundary layer forms the pigment layer containing the laser-sensitive pigment.
  • the boundary layer has a thickness of 2 ⁇ m to 5 ⁇ m.
  • Suitable additives are in particular color pigments and metal salts.
  • pigments of Firm TherMark find use, for example TherMark 120-30F, which are metal oxides, for example molybdenum trioxide.
  • mixtures of several pigments or blends of pigments and glass particles, such as are available from Merck can be used, which can lead to a sintering process.
  • the additive can be used in addition to the additive titanium dioxide.
  • additives are added to the suspension to form the layer (such as in DE G 81 30 861 described) in particular of the order of a few parts per thousand to a maximum of 10 percent, preferably in amounts of 0.1 to 10 wt .-%, in particular from 0.5 to 6 wt .-% based on the total weight of the layer, admixed, namely most advantageously in concentrations of 0.5% by weight, 1% by weight, and 2.5% by weight and 4% by weight.
  • the laser beam penetrates through the carrier layer and the adhesive layer and strikes the pigment.
  • the energy is absorbed, and there is a sublimation process in which the pigment is transferred to the substrate and forms a permanent and stable bond with the substrate. It will get sharp, high-contrast labels and markings.
  • the known direct and indirect application methods are suitable.
  • Acrylic hotmelts can be applied to the mentioned supports in addition to the standard application methods such as direct coating from nozzles, over rollers and the like. also apply in the transfer process, as under DE 43 24 748 C2 be revealed.
  • the adhesive is first applied to an endlessly circulating, antiadhesive equipped Gurtband and then transferred in a laminating station, if necessary using pressure and temperature to improve the Masseverank réelle- on the carrier material.
  • an application of the adhesive from organic solvents or as an aqueous dispersion is possible;
  • the economic and environmental benefits of the hotmelt dosage form are obvious.
  • the adhesive and the layer containing the laser-sensitive pigment can be screen-dot-like by screen printing (FIG. DE 42 37 252 C2 ), wherein the adhesive dots may also be distributed differently and / or differently ( EP 0 353 972 B1 ), by gravure ( DE 43 08 649 C2 ) are applied in longitudinal and transverse contiguous webs, by screen printing or by flexographic printing.
  • Both layers may preferably be in dome form by screen printing or applied in a different pattern such as grids, stripes, zigzag lines and, for example, by gravure. Furthermore, it can also be sprayed on, for example, which results in a more or less irregular application pattern.
  • these are applied in the form of polygeometric calottes.
  • the calottes can have different shapes. Preferred are flattened hemispheres.
  • the printing of other shapes and patterns on the substrate is possible, such as a printed image in the form of alphanumeric character combinations or patterns such as grids, stripes, the further accumulation of calotte and zigzag lines.
  • aspired porous adhesive coating is for the subject invention as homogeneous, smooth, air-free and impermeable adhesive coating advantage. If instead of the above-described structured surface, however, a smooth and homogeneous surface of the intermediate carrier is selected, these requirements can be met.
  • the basic body for the intermediate carrier can be chosen from all common materials for such purposes. Woven webbings made of glass fiber, polyester, polyamide or Nomex®, a fiber material from DuPont, are particularly advantageous. But also blankets, plastic straps and the like have been found to be favorable. When fabric tapes are selected, it is beneficial to use those already provided with a substantially unstructured plastic surface finish. This latter coating promotes the adhesion and uniformity of the actual surface coating on the body. The surface coating itself ensures the desired easy transfer of the adhesive mass from the intermediate carrier to the final carrier.
  • this surface of the intermediate carrier is coated with an anti-adhesive layer, for example, of crosslinked silicone rubber or fluoropolymers such as Teflon®.
  • the laser transfer film according to the invention exhibits excellent properties, in particular much better, than the transfer films which have laser-sensitive pigments in a homogeneous distribution within the adhesive layer.
  • the adhesive can be greatly adversely affected in its temporary adhesive property (Klebmasseumspulungen) and in the transfer of the pigments in or on the component.
  • the film according to the invention does not show the negative effects on coatings and plastic sheets (PP) due to the pigmented boundary layer to the bonding component, but a permanent inscription on the component.
  • a very good labeling result is achieved. It also shows a surprisingly low level of smoke.
  • the lettering showed a slightly wider but strongly high-contrast lettering directly after the lettering. After a polish, the contrast diminishes a little, but the contours of the font become a little sharper.
  • the film of the invention can be used outstandingly the film of the invention, such as on ceramic base of fuses the company Osram or generally on glass.
  • the advantages come into their own, the label can be applied to the component and laser-engraved. After the lettering it will be deducted. The process is finished.
  • the laser transfer film according to the invention can be wound as an endless roll, this in the form of an Archimedean spiral around mostly a cardboard tube, and as a punched Be offered label.
  • the latter can have any desired shape, perfectly adapted to the particular application.
  • FIG. 1 the construction of a film according to the invention in the form of a label is shown.
  • the film is composed of the carrier layer 1, the first adhesive view 2, which is applied over the entire area to the carrier material 1 and composed of the layer 3 containing the laser-sensitive pigment.
  • the layer 3 is also applied over the entire surface.
  • FIG. 2 shows the structure of a film according to the invention in the form of a label, wherein in addition a second adhesive view 4 is applied.
  • This adhesive layer has been applied only partially in the form of individual calottes. These serve as breakpoints or positioning of the film on the ground.
  • the FIG. 3 discloses the process of labeling a component 5 using the film of the invention.
  • the laser transfer film preferably in the form of a label, applied to the component 5, wherein through the adhesive layer 2 a Liability and fixation of the label is achieved.
  • the labeling is carried out by means of a laser, which is indicated by the red cylinder.
  • the transfer film is removed on the component remains the desired label 6 back.

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Adhesive Tapes (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Laminated Bodies (AREA)
  • Decoration By Transfer Pictures (AREA)

Claims (9)

  1. Feuille de transfert par laser pour une inscription durable sur des pièces, constituée d'au moins une couche support, une couche adhésive étant présente sur toute la surface de la face inférieure de la couche support, la couche support et la couche adhésive étant transparentes ou translucides et n'absorbant pas un rayonnement laser, caractérisée en ce qu'une couche de pigment est appliquée sur toute la surface de la face inférieure de la couche adhésive, contenant au moins un pigment sensible au laser, qui absorbe l'énergie d'un rayon laser et qui sublime.
  2. Feuille de transfert par laser selon la revendication 1, caractérisée en ce que la structure de base de la couche de pigment contenant les pigments sensibles au laser est également constituée par l'adhésif de la couche adhésive.
  3. Feuille de transfert par laser selon la revendication 1 ou 2, caractérisée en ce qu'une deuxième couche adhésive est appliquée sur la couche de pigment contenant le pigment sensible au laser.
  4. Feuille de transfert par laser selon au moins l'une quelconque des revendications 1 à 3, caractérisée en ce qu'on utilise comme matériau support des feuilles, en particulier des feuilles étirées monoaxialement et biaxialement à base de polyoléfines, puis des feuilles à base de polyéthylène étiré ou de copolymères étirés, contenant des unités d'éthylène et/ou de polypropylène, le cas échéant également des feuilles en PVC, des feuilles en PET, des feuilles à base de polymères de vinyle, de polyamides, de polyesters, de polyacétals, de polycarbonates, de manière tout particulièrement préférée des feuilles transparentes.
  5. Feuille de transfert par laser selon au moins l'une quelconque des revendications 1 à 4, caractérisée en ce qu'on utilise comme couche adhésive une masse auto-adhésive à base de caoutchouc naturel, de PUR, d'acrylates ou de copolymères à blocs de styrène-isoprène-styrène.
  6. Feuille de transfert par laser selon les revendications 1 à 5, caractérisée en ce que des pigments colorés et des sels métalliques, en particulier des oxydes métalliques, ainsi que des mélanges de différents pigments avec des particules de verre sont incorporés dans la couche de pigments.
  7. Utilisation d'une feuille de transfert par laser selon au moins l'une quelconque des revendications 1 à 6 pour l'application d'une inscription durable sur du verre, de la céramique et/ou du métal.
  8. Utilisation d'une feuille de transfert par laser selon au moins l'une quelconque des revendications 1 à 6 pour l'application d'une inscription durable sur des laquages et des plaques en matériau synthétique.
  9. Utilisation d'une feuille de transfert par laser selon au moins l'une quelconque des revendications 1 à 6 comme étiquette découpée.
EP02781201A 2001-10-25 2002-10-02 Film de transfert par laser pour etiquetage durable d'elements constitutifs Expired - Lifetime EP1449186B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10152073A DE10152073A1 (de) 2001-10-25 2001-10-25 Laser-Transferfolie zum dauerhaften Beschriften von Bauteilen
DE10152073 2001-10-25
PCT/EP2002/011023 WO2003035411A2 (fr) 2001-10-25 2002-10-02 Film de transfert par laser pour etiquetage durable d'elements constitutifs

Publications (2)

Publication Number Publication Date
EP1449186A2 EP1449186A2 (fr) 2004-08-25
EP1449186B1 true EP1449186B1 (fr) 2011-08-31

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EP02781201A Expired - Lifetime EP1449186B1 (fr) 2001-10-25 2002-10-02 Film de transfert par laser pour etiquetage durable d'elements constitutifs

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US (1) US6764803B2 (fr)
EP (1) EP1449186B1 (fr)
AT (1) ATE522898T1 (fr)
AU (1) AU2002349320A1 (fr)
DE (1) DE10152073A1 (fr)
ES (1) ES2370814T3 (fr)
WO (1) WO2003035411A2 (fr)

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AU2002349320A1 (en) 2003-05-06
EP1449186A2 (fr) 2004-08-25
US20030104309A1 (en) 2003-06-05
WO2003035411A3 (fr) 2003-10-23
US6764803B2 (en) 2004-07-20
WO2003035411A2 (fr) 2003-05-01
DE10152073A1 (de) 2003-05-08
ES2370814T3 (es) 2011-12-23
ATE522898T1 (de) 2011-09-15

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