EP0774365A1 - Process for decorating composite articles such as skis, surfboards or skateboards - Google Patents
Process for decorating composite articles such as skis, surfboards or skateboards Download PDFInfo
- Publication number
- EP0774365A1 EP0774365A1 EP96115909A EP96115909A EP0774365A1 EP 0774365 A1 EP0774365 A1 EP 0774365A1 EP 96115909 A EP96115909 A EP 96115909A EP 96115909 A EP96115909 A EP 96115909A EP 0774365 A1 EP0774365 A1 EP 0774365A1
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- European Patent Office
- Prior art keywords
- decoration
- sheet
- hot
- layer
- contrast
- 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.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B44—DECORATIVE ARTS
- B44C—PRODUCING DECORATIVE EFFECTS; MOSAICS; TARSIA WORK; PAPERHANGING
- B44C1/00—Processes, not specifically provided for elsewhere, for producing decorative surface effects
- B44C1/16—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like
- B44C1/165—Processes, not specifically provided for elsewhere, for producing decorative surface effects for applying transfer pictures or the like for decalcomanias; sheet material therefor
- B44C1/17—Dry transfer
- B44C1/1712—Decalcomanias applied under heat and pressure, e.g. provided with a heat activable adhesive
- B44C1/1716—Decalcomanias provided with a particular decorative layer, e.g. specially adapted to allow the formation of a metallic or dyestuff layer on a substrate unsuitable for direct deposition
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- A—HUMAN NECESSITIES
- A63—SPORTS; GAMES; AMUSEMENTS
- A63C—SKATES; SKIS; ROLLER SKATES; DESIGN OR LAYOUT OF COURTS, RINKS OR THE LIKE
- A63C5/00—Skis or snowboards
- A63C5/003—Structure, covering or decoration of the upper ski surface
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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
- B41M5/025—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet
- B41M5/035—Duplicating or marking methods; Sheet materials for use therein by transferring ink from the master sheet by sublimation or volatilisation of pre-printed design, e.g. sublistatic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M7/00—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
- B41M7/0027—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock using protective coatings or layers by lamination or by fusion of the coatings or layers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/2481—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including layer of mechanically interengaged strands, strand-portions or strand-like strips
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/24843—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] with heat sealable or heat releasable adhesive layer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/24917—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including metal layer
Definitions
- the invention relates to a new method of decorating a composite article. It relates more particularly to articles in the form of laminates comprising different plastic and composite materials such as skis in general, surfboards, skateboards and other objects of a similar nature.
- Sublimation is a technique well suited for decorating skis, which makes it possible to use many different plastic supports and to print any patterns without it being necessary to subject the support to a preliminary specific preparation operation.
- the transfer principle consists in evaporating inks contained on a support paper in the form of dry extracts by application of heat and pressure against the support to be decorated. The process is clean, fast and free from harmful vapors or solvents.
- the decoration is transferred to the external surface of a transparent layer covering the article to be decorated.
- An ink gradient forms over a few tenths of a mm from the external surface towards the interior of the transparent layer.
- the major drawback is that the decoration is directly subjected to external aggressions and can be deteriorated quickly if the conditions of use of the article are severe (when the article is subjected to shocks, scratches, significant UV radiation, etc., by example).
- Patent application FR-A-2 620 975 also belonging to the applicant is distinguished from the previous one by the fact that the sublimation takes place first on an opaque monolayer sheet which is then assembled by gluing on a transparent monolayer sheet of protection. The assembly is then attached to the article by hot gluing.
- the transparent layer thus decorated is assembled with an opaque layer.
- the assembly is then secured to the composite article by hot bonding.
- the increase in temperature during bonding causes a restart of the migration of the inks, which then diffuse in the opaque layer.
- Deep diffusion creates the aforementioned pastellization problem, which is also associated with significant lateral diffusion due to a certain heat creep of the opaque layer; which makes the final decor less clear.
- the Applicant has provided a satisfactory solution to this problem of migration of inks which is set out in unpublished French Application No. 95 00684. It consists in covering the sublimed transparent layer with a transparent coating of crosslinkable material and then proceeding to crosslinking hardening of the coating to improve its creep resistance and thermal stability. This process does not only have advantages.
- the layer of crosslinkable material is preferably chosen from varnishes. It is also necessary to apply a layer of white lacquer or a contrasting color over the layer of crosslinkable material.
- the object of the present invention is to provide a solution to the aforementioned problems.
- one of the goals is to offer a decoration solution by internal sublimation which is more ecological by avoiding the use of materials such as solvents, thinners and other products of the same nature.
- Another object of the invention is in addition to enhancing the decoration patterns by very diverse and attractive material effects, such as, for example, a metallic, woven, screened background effect, etc.
- Sublimation inks do not have the possibility of migrating into different materials during the final cycle. Thus, the decor remains clean and retains its original colors. These different materials also make it possible to obtain particularly striking and varied background effects.
- the contrast sheet is a non-anodized aluminum sheet covered on each side with a film of an olefin copolymer of the ionomer type.
- the film serves as a bonding interface and makes aluminum compatible with bonding with most of the substrates with which it is intended to adhere. It also serves as protection against oxidation of the aluminum foil during storage thereof.
- a barrier film is approached on the face of the contrast sheet of natural or synthetic dry fiber material, intended to come into contact with the flowable resin of the reinforcement structure of the article; said barrier film being chosen from a material having good bonding compatibility with the contrast sheet on the one hand and with the hot-melt resin on the other hand. This avoids the resin of the reinforcing structure from crossing or impregnating the contrast sheet and consequently creating appearance defects visible externally (phenomena of bubbles, stains, etc.).
- the barrier film comes into contact with the heat and pressure exerted during the second assembly cycle of the contrast sheet on the plastic layer.
- the invention also relates to the decoration complex intended to be assembled with a reinforcing structure based on hot-melt resin of a composite article.
- Figure 1 shows the first sublimation transfer cycle of the process of the invention.
- FIGS 2 and 3 show the second cycle of hot assembly and pressure of the process of the invention.
- Figure 4 shows a schematic sectional view of a ski covered with the complex of the invention.
- Figure 5 is a view similar to Figure 2 according to a variant of the invention.
- Carrying out the method according to the invention requires first of all the use of a monolayer plastic sheet 1 made of transparent or translucent material; this sheet will be called “transparent layer” in the description below.
- a decoration is printed by transfer of sublimable dyes.
- This face 100 is intended to constitute the internal side of the transparent layer in the complex; as opposed to the opposite face 101 which is the outer side.
- the decoration pattern to be printed is in a manner known per se contained in a sheet of support paper 4 which is applied under a pressure P at a temperature T for a time t against the face 100 of the transparent layer.
- the transparent layer can be chosen from the sublimable plastics of polyamides such as PA11, PA12, PA6.3, PA6.6, etc., Polycarbonates, ABS (Acrylonitrile Butadiene Styrene), transparent AS (Acrylonitrile Styrene) mixed with TPU (Thermoplastic Urethane Elastomer), Polyethylene Terephthalates (PET).
- polyamides such as PA11, PA12, PA6.3, PA6.6, etc.
- Polycarbonates ABS (Acrylonitrile Butadiene Styrene), transparent AS (Acrylonitrile Styrene) mixed with TPU (Thermoplastic Urethane Elastomer), Polyethylene Terephthalates (PET).
- the thickness of the transparent layer is between 0.2 and 1.1 mm. Sublimation is carried out at a temperature between 160 and 180 ° C, a pressure of 1 to 2 bars for a time between 1mn30sec and 4mn approximately. The depth of the ink migration front through the transparent layer on the internal side is of the order or slightly greater than 0.20 mm.
- this transparent layer 1 is brought together with a solid bonding film 2 and a contrast layer 3.
- the bonding film 2 is brought into contact with the predecorated face 100 and the contrast layer 3 is brought into contact with the bonding film (FIG. 2).
- an actual plating phase is carried out by increasing the pressure and temperature up to at least the softening point of the film, in order to obtain adhesion of the transparent layer 1 with the contrast layer 3.
- the contrast layer is a thin, non-anodized aluminum sheet 31 covered on each side with a film of an olefin copolymer of the ionomer type (trade name SURLYN®).
- the thickness of the aluminum foil is between 15 and 60 ⁇ m thick and the thickness of each film between 10 and 50 ⁇ m.
- the bonding film is chosen for its adhesion power with the transparent layer 1 and with the contrast layer 3. It is a hot-melt film of thin thickness between a few microns and a few tenths of a millimeter.
- a film 2 based on polymer or copolymer grafted by the action of carboxylic acid or carboxylic acid anhydride for example by acrylic acid, by methacrylic acid, or by maleic anhydride.
- Such a film 2 can in particular be produced from grafted polyethylene, for example from polyethylene grafted with maleic anhydride.
- This nature of film allows the bonding of most of the sublimable materials constituting the transparent layer 1 mentioned above with the contrast layer of aluminum treated ionomer.
- film 2 can also consist of a copolymer of ethylene and vinyl acetate (EVA), grafted by the action of carboxylic acid or carboxylic acid anhydride.
- EVA ethylene and vinyl acetate
- the use of a polyethylene film 2 grafted with maleic anhydride allows the bonding of a first polyamide element 1 on a contrast layer 3 of aluminum ionomer treated.
- the film 2 is caused to adhere to the first element 1 by chemical reaction between the maleic anhydride groups grafted on the surface of the polyethylene and the end groups of the polyamide. These groups exist in low concentration in the material, but have the particularity of migrating to the extreme surface during the extrusion of the polyamide sheet and are therefore available for the reaction.
- the reaction leads to the substitution of the oxygen atom of the maleic cycle by the nitrogen atom of the amino terminal group of the polyamide and formation of a water molecule. It is necessary to bring the substrates to temperatures above 110 ° C to trigger the reaction.
- the film 6 must therefore be pressed hot, by calendering or pressing, against the first element 1 to ensure that they join together.
- the various layers 1, 2, 3 are assembled in the context of a single heating and pressurization cycle.
- the complex thus formed is then ready for use to serve for covering a composite article to be decorated.
- composite article is meant essentially any laminated object having a reinforcing structure. We think in particular of skis, snowboards, skateboards, etc.
- Figure 4 schematically shows the section of a ski which comprises a complex obtained according to the method of the invention.
- connection of the complex with the rest of the ski structure can be done in very different processes.
- a hot pressing cycle is generally carried out with the reinforcement structure 4 of the ski based on thermofluable resin.
- This reinforcing structure 4 may in particular consist of a reinforcing textile sheet pre-impregnated with a thermosetting resin or a thermoplastic resin.
- thermosetting resin chosen from the group consisting of polyester, epoxides, polyurethanes .
- thermoplastic resin chosen from the group consisting of polyamides, polycarbonates, PEI (Polyether Imide).
- the contrast sheet 3 can be chosen from the group consisting of non-anodized aluminum, synthetic dry fiber and wood.
- the contrast sheet is made of dry fibers, it is advantageously in the form of a nonwoven or woven textile sheet (or veil) made of glass fibers, carbon, polyester, polyaramide or other synthetic or natural fibers, such as cotton for example.
- the bonding film 20 plays an important role in buffering sublimation inks which tend to want to migrate naturally into the layer of dry fiber 3.
- the barrier film 21 as to it is chosen from a material having good bonding compatibility with the contrast sheet 3, on the one hand, and with the hot-melt resin of the reinforcement structure of the composite article to be decorated, on the other hand.
- the barrier film can also be docked during the final assembly of the complex with the reinforcing structure of the article to be decorated during the subsequent hot pressing cycle.
- the barrier film 21 can be made of a thermoformable material such as an ionomer material, preferably tinted in the mass to improve the contrast of the sheet 3.
- the barrier film is chosen from a material whose viscosity is such that it penetrates inside the fiber interstices and mouths.
- Another advantage of the dry fiber lies in its ability to prevent, as much, the lateral creep of the bonding film 20. During the hot assembly cycle, the fiber absorbs part of the molten thermoplastic material due to its porosity. .
- an ionomer barrier film allows the bonding of a contrast sheet chosen from the materials mentioned above with the reinforcement structure based on thermofluidable resin of the epoxy type.
Landscapes
- Laminated Bodies (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
Description
L'invention concerne un nouveau procédé de décoration d'un article composite. Elle se rapporte plus particulièrement aux articles se présentant sous la forme de stratifiés regroupant différents matériaux plastiques et composites tels que les skis en général, les surfs, les planches à roulette et autres objets de nature similaire.The invention relates to a new method of decorating a composite article. It relates more particularly to articles in the form of laminates comprising different plastic and composite materials such as skis in general, surfboards, skateboards and other objects of a similar nature.
La sublimation est une technique bien adaptée pour la décoration des skis, qui permet d'utiliser de nombreux supports plastiques différents et d'imprimer des motifs quelconques sans qu'il soit nécessaire de soumettre le support à une opération préliminaire de préparation spécifique. Le principe de transfert consiste à faire évaporer des encres contenues sur un papier support sous forme d'extraits secs par application de chaleur et de pression contre le support à décorer. Le procédé est propre, rapide et sans émanation de vapeurs ou de solvants nocifs.Sublimation is a technique well suited for decorating skis, which makes it possible to use many different plastic supports and to print any patterns without it being necessary to subject the support to a preliminary specific preparation operation. The transfer principle consists in evaporating inks contained on a support paper in the form of dry extracts by application of heat and pressure against the support to be decorated. The process is clean, fast and free from harmful vapors or solvents.
Dans la plupart des cas, le décor est transféré sur la surface externe d'une couche transparente recouvrant l'article à décorer. Un gradient d'encre se forme sur quelques dixièmes de mm à partir de la surface externe vers l'intérieur de la couche transparente. L'inconvénient majeur est que le décor est directement soumis aux agressions extérieures et peut être détérioré rapidement si les conditions d'utilisation de l'article sont sévères (lorsque l'article est soumis aux chocs, éraflures, rayonnement U.V. important, etc, par exemple).In most cases, the decoration is transferred to the external surface of a transparent layer covering the article to be decorated. An ink gradient forms over a few tenths of a mm from the external surface towards the interior of the transparent layer. The major drawback is that the decoration is directly subjected to external aggressions and can be deteriorated quickly if the conditions of use of the article are severe (when the article is subjected to shocks, scratches, significant UV radiation, etc., by example).
On a tenté d'apporter des solutions à ces problèmes comme par exemple dans la demande de brevet FR-A-2 620 974 appartenant à la demanderesse où l'on propose de réaliser la sublimation à travers une couche interne opaque solidarisée préalablement par extrusion avec une couche externe transparente. Le bicouche ainsi décoré est ensuite rapporté puis solidarisé sur l'article.We have tried to provide solutions to these problems as for example in patent application FR-A-2 620 974 belonging to the applicant where it is proposed to carry out the sublimation through an opaque internal layer previously secured by extrusion with a transparent outer layer. The bilayer thus decorated is then attached and then secured to the article.
La demande de brevet FR-A-2 620 975 appartenant également à la demanderesse se distingue de la précédente par le fait que la sublimation s'effectue d'abord sur une feuille monocouche opaque qui est ensuite assemblée par collage sur une feuille monocouche transparente de protection. L'ensemble est ensuite rapporté sur l'article par collage à chaud.Patent application FR-A-2 620 975 also belonging to the applicant is distinguished from the previous one by the fact that the sublimation takes place first on an opaque monolayer sheet which is then assembled by gluing on a transparent monolayer sheet of protection. The assembly is then attached to the article by hot gluing.
Dans ces deux cas, la migration des encres se fait à travers de la couche opaque ; ce qui crée une perte dans la définition finale du décor. Même si le front de migration plus concentré en encre apparaît, on obtient une pastellisation du décor, due à la diffusion verticale des encres au travers de la couche opaque.In these two cases, the migration of the inks takes place through the opaque layer; which creates a loss in the final definition of the decor. Even if the migration front more concentrated in ink appears, the decoration is pastellized, due to the vertical diffusion of the inks through the opaque layer.
D'autres solutions ont été essayées comme par exemple de réaliser la sublimation à travers la face interne de la couche transparente de protection.Other solutions have been tried, such as, for example, carrying out the sublimation through the internal face of the transparent protective layer.
La couche transparente ainsi décorée, est assemblée avec une couche opaque. L'ensemble est ensuite solidarisé sur l'article composite par collage à chaud. Dans ce cas, l'augmentation de la température lors du collage provoque un redémarrage de la migration des encres, qui diffusent alors dans la couche opaque. La diffusion en profondeur crée le problème de pastellisation précité, auquel est également associé une diffusion latérale importante en raison d'un certain fluage à la chaleur de la couche opaque ; ce qui rend le décor final moins net.The transparent layer thus decorated is assembled with an opaque layer. The assembly is then secured to the composite article by hot bonding. In in this case, the increase in temperature during bonding causes a restart of the migration of the inks, which then diffuse in the opaque layer. Deep diffusion creates the aforementioned pastellization problem, which is also associated with significant lateral diffusion due to a certain heat creep of the opaque layer; which makes the final decor less clear.
La demanderesse a apporté une solution satisfaisante à ce problème de migration des encres qui est exposée dans la demande française non publiée n° 95 00684. Elle consiste à procéder au recouvrement de la couche transparente sublimée par un revêtement transparent en matière réticulable et ensuite procéder au durcissement par réticulation du revêtement pour améliorer sa résistance au fluage et sa stabilité thermique. Ce procédé ne comporte pas que des avantages.The Applicant has provided a satisfactory solution to this problem of migration of inks which is set out in unpublished French Application No. 95 00684. It consists in covering the sublimed transparent layer with a transparent coating of crosslinkable material and then proceeding to crosslinking hardening of the coating to improve its creep resistance and thermal stability. This process does not only have advantages.
En particulier, la couche de matière réticulable est choisie, de préférence, parmi les vernis. Il est nécessaire aussi d'appliquer une couche de laque blanche ou de couleur contrastée par dessus la couche de matière réticulable.In particular, the layer of crosslinkable material is preferably chosen from varnishes. It is also necessary to apply a layer of white lacquer or a contrasting color over the layer of crosslinkable material.
Ces produits contiennent des solvants ou diluants fortement volatiles, inflammables et souvent nocifs. Leur application en toute sécurité pour la santé des manipulateurs et pour l'environnement en général, réclament l'emploi de moyens spécifiques.These products contain highly volatile, flammable and often harmful solvents or diluents. Their application in complete safety for the health of the manipulators and for the environment in general, requires the use of specific means.
De plus, il faut aussi respecter des temps de séchage ou employer des moyens adaptés de réticulation rapide comme le rayonnement U.V., par exemple. La plupart du temps, il est aussi nécessaire d'opérer des traitements de surface pour améliorer l'adhésion entre les différentes couches.In addition, it is also necessary to respect drying times or to employ suitable means of rapid crosslinking such as UV radiation, for example. Most of the time, it is also necessary to operate surface treatments to improve the adhesion between the different layers.
D'une manière plus générale aussi ; en raison de la présence d'une couche de contraste en plastique ou d'une laque, les effets de fond sont peu variés et conduisent tous à un rendu assez semblable.In a more general way too; due to the presence of a plastic contrast layer or a lacquer, the background effects are not very varied and all lead to a fairly similar rendering.
L'objet de la présente invention est d'apporter une solution aux problèmes précités.The object of the present invention is to provide a solution to the aforementioned problems.
En particulier, l'un des buts est de proposer une solution de décoration par sublimation interne qui soit plus écologique en évitant l'emploi de matières telles que les solvants, diluants et autres produits de même nature.In particular, one of the goals is to offer a decoration solution by internal sublimation which is more ecological by avoiding the use of materials such as solvents, thinners and other products of the same nature.
Un autre but de l'invention est en plus de mettre en valeur les motifs de décoration par des effets de matière très diversifiés et attractifs, comme par exemple, un effet de fond métallisé, tissé, tramé, etc.Another object of the invention is in addition to enhancing the decoration patterns by very diverse and attractive material effects, such as, for example, a metallic, woven, screened background effect, etc.
Pour cela l'invention concerne un procédé de décoration d'un article composite comprenant la préparation d'un complexe décoré pour être assemblé avec une structure de renfort de l'article à base de résine fluable à chaud lors d'un cycle ultérieur de pressage à chaud. Il comprend :
- un premier cycle, au cours duquel on effectue le transfert d'un décor par la méthode d'impression d'encre(s) sublimable(s) sur la première face d'une couche de matière plastique transparente ou translucide ;
- on procède ensuite dans un second cycle au moyen d'un film de collage à l'assemblage à chaud et sous pression sur la première face ainsi décorée, d'une feuille de contraste en matériau choisi parmi le groupe constitué par l'aluminium non anodisé, la fibre sèche synthétique, le bois.
- a first cycle, during which a decoration is transferred by the printing method of sublimable ink (s) on the first face of a transparent or translucent plastic layer;
- we then proceed in a second cycle by means of a bonding film to the hot assembly and under pressure on the first face thus decorated, of a contrast sheet of material chosen from the group consisting of non-anodized aluminum , synthetic dry fiber, wood.
Les encres de sublimation n'ont pas la possibilité de migrer dans les différents matériaux lors du cycle final. Ainsi, le décor reste net et conserve ses couleurs d'origine. Ces différents matériaux permettent aussi d'obtenir des effets de fond particulièrement saisissants et variés.Sublimation inks do not have the possibility of migrating into different materials during the final cycle. Thus, the decor remains clean and retains its original colors. These different materials also make it possible to obtain particularly striking and varied background effects.
Selon une autre caractéristique de l'invention, la feuille de contraste est une feuille aluminium non anodisée recouverte sur chaque face d'une pellicule d'un copolymère d'oléfine du type ionomère. La pellicule sert d'interface de collage et rend l'aluminium compatible au collage avec la plupart des substrats avec lesquels il est destiné à adhérer. Elle sert aussi de protection contre une oxydation de la feuille d'aluminium lors du stockage de celle-ci.According to another characteristic of the invention, the contrast sheet is a non-anodized aluminum sheet covered on each side with a film of an olefin copolymer of the ionomer type. The film serves as a bonding interface and makes aluminum compatible with bonding with most of the substrates with which it is intended to adhere. It also serves as protection against oxidation of the aluminum foil during storage thereof.
Selon une autre caractéristique, on procède à l'accostage d'un film barrière sur la face de la feuille de contraste en matériau de fibres sèches naturelles ou synthétiques, destinée à entrer en contact avec la résine fluable de la structure de renfort de l'article ; ledit film barrière étant choisi dans un matériau ayant une bonne compatibilité de collage avec la feuille de contraste d'une part et avec la résine fluable à chaud d'autre part. On évite ainsi à la résine de la structure de renfort de traverser ou d'imprégner la feuille de contraste et de créer par conséquent, des défauts d'aspect visibles extérieurement (phénomènes de bulles, tâches...etc).According to another characteristic, a barrier film is approached on the face of the contrast sheet of natural or synthetic dry fiber material, intended to come into contact with the flowable resin of the reinforcement structure of the article; said barrier film being chosen from a material having good bonding compatibility with the contrast sheet on the one hand and with the hot-melt resin on the other hand. This avoids the resin of the reinforcing structure from crossing or impregnating the contrast sheet and consequently creating appearance defects visible externally (phenomena of bubbles, stains, etc.).
Selon une caractéristique liée à la précédente, l'accostage du film barrière se fait en profitant de la chaleur et pression exercée pendant le second cycle d'assemblage de la feuille de contraste sur la couche de matière plastique.According to a characteristic linked to the previous one, the barrier film comes into contact with the heat and pressure exerted during the second assembly cycle of the contrast sheet on the plastic layer.
Dans une solution alternative, on peut aussi prévoir que l'accostage du film barrière se fasse pendant l'assemblage final du complexe décoré avec la structure de renfort de l'article lors du cycle ultérieur de pressage à chaud.In an alternative solution, provision can also be made for the barrier film to be docked during the final assembly of the decorated complex with the reinforcing structure of the article during the subsequent hot pressing cycle.
L'invention concerne aussi le complexe de décoration destiné à être assemblé avec une structure de renfort à base de résine fluable à chaud d'un article composite.The invention also relates to the decoration complex intended to be assembled with a reinforcing structure based on hot-melt resin of a composite article.
D'autres caractéristiques et avantages de l'invention se dégageront de la description qui va suivre en regard des dessins annexés qui ne sont donnés qu'à titre d'exemples non limitatifs.Other characteristics and advantages of the invention will emerge from the description which follows with reference to the appended drawings which are given only by way of nonlimiting examples.
La figure 1 montre le premier cycle de transfert par sublimation du procédé de l'invention.Figure 1 shows the first sublimation transfer cycle of the process of the invention.
Les figures 2 et 3 montrent le second cycle d'assemblage à chaud et sous pression du procédé de l'invention.Figures 2 and 3 show the second cycle of hot assembly and pressure of the process of the invention.
La figure 4 montre une vue schématiquement en coupe d'un ski recouvert du complexe de l'invention.Figure 4 shows a schematic sectional view of a ski covered with the complex of the invention.
La figure 5 est une vue similaire à la figure 2 selon une variante de l'invention.Figure 5 is a view similar to Figure 2 according to a variant of the invention.
La réalisation du procédé selon l'invention requiert tout d'abord l'utilisation d'une feuille plastique monocouche 1 en matériau transparent ou translucide ; cette feuille sera dénommée "couche transparente" dans la description ci-après.Carrying out the method according to the invention requires first of all the use of a monolayer
Sur l'une des faces 100 de la couche 1, on procède, dans une première étape, à une impression d'un décor par transfert de colorants sublimables. Cette face 100 est destinée à constituer le côté interne de la couche transparente dans le complexe ; par opposition à la face opposée 101 qui est le côté externe. Le motif de décoration à imprimer est de façon connue en soi contenu dans une feuille de papier support 4 qui est appliquée sous une pression P à une température T pendant un temps t contre la face 100 de la couche transparente. La couche transparente peut être choisie parmi les matières plastiques sublimables de Polyamides tels que les PA11, PA12, PA6.3, PA6.6, etc, les Polycarbonates, les ABS (Acrylonitrile Butadiène Styrène), les AS (Acrylonitrile Styrène) transparents mélangés à un TPU (Elastomère thermoplastique uréthane), les Polyéthylènes Téréphtalates (PET).On one of the
L'épaisseur de la couche transparente est comprise entre 0,2 et 1,1 mm. La sublimation est opérée à une température comprise entre 160 et 180°C, une pression de 1 à 2 bars pendant un temps compris entre 1mn30sec et 4mn environ. La profondeur du front de migration des encres au travers de la couche transparente du côté interne est de l'ordre ou légèrement supérieur à 0,20 mm.The thickness of the transparent layer is between 0.2 and 1.1 mm. Sublimation is carried out at a temperature between 160 and 180 ° C, a pressure of 1 to 2 bars for a time between 1mn30sec and 4mn approximately. The depth of the ink migration front through the transparent layer on the internal side is of the order or slightly greater than 0.20 mm.
Au cours d'une seconde étape, on effectue le rapprochement de cette couche transparente 1 avec un film solide de collage 2 et une couche de contraste 3. Le film de collage 2 est mis en contact avec la face prédécorée 100 et la couche de contraste 3 est mise en contact avec le film de collage (figure 2).During a second step, this
On procède ensuite à une phase de plaquage proprement dit par augmentation de pression et température jusqu'au point de ramollissement au moins du film, afin d'obtenir l'adhésion de la couche transparente 1 avec la couche de contraste 3.Next, an actual plating phase is carried out by increasing the pressure and temperature up to at least the softening point of the film, in order to obtain adhesion of the
Dans l'exemple illustré, la couche de contraste est une feuille d'aluminium non anodisée de fine épaisseur 31 recouverte sur chaque face d'une pellicule d'un copolymère d'oléfine du type ionomère (nom commercial SURLYN®).In the example illustrated, the contrast layer is a thin,
L'épaisseur de la feuille d'aluminium est comprise entre 15 et 60 µm d'épaisseur et l'épaisseur de chaque pellicule comprise entre 10 et 50 µm.The thickness of the aluminum foil is between 15 and 60 µm thick and the thickness of each film between 10 and 50 µm.
Le film de collage est choisi pour son pouvoir d'adhérence avec la couche transparente 1 et avec la couche de contraste 3. Il s'agit d'un film thermofusible de fine épaisseur comprise entre quelques microns et quelques dixièmes de millimètres.The bonding film is chosen for its adhesion power with the
On peut avantageusement utiliser un film 2 à base de polymère ou copolymère greffé par action d'acide carboxylique ou d'anhydride d'acide carboxylique, par exemple par l'acide acrylique, par l'acide méthacrylique, ou par l'anhydride maléique.It is advantageous to use a
Un tel film 2 peut notamment être réalisé en polyéthylène greffé, par exemple en polyéthylène greffé par l'anhydride maléique.Such a
Cette nature de film permet le collage de la plupart des matériaux sublimables constituant la couche transparente 1 cités précédemment avec la couche de contraste en aluminium traitée ionomère.This nature of film allows the bonding of most of the sublimable materials constituting the
Mais le film 2 peut aussi être constitué d'un copolymère d'éthylène et d'acétate de vinyle (EVA), greffé par action d'acide carboxylique ou d'anhydride d'acide carboxylique.However,
A titre d'exemple, l'utilisation d'un film 2 en polyéthylène greffé à l'anhydride maléique permet le collage d'un premier élément 1 en polyamide sur une couche de contraste 3 aluminium traité ionomère. Selon l'invention, on provoque l'adhésion du film 2 sur le premier élément 1 par réaction chimique entre les groupements anhydride maléique greffés à la surface du polyéthylène et les groupements terminaux du polyamide. Ces groupements existent en faible concentration dans le matériau, mais présentent la particularité de migrer à l'extrême surface lors de l'extrusion de la feuille de polyamide et sont donc disponibles pour la réaction. La réaction conduit à la substitution de l'atome d'oxygène du cycle maléique par l'atome d'azote du groupement terminal amine du polyamide et formation d'une molécule d'eau. Il est nécessaire de porter les substrats à des températures supérieures à 110°C pour déclencher la réaction. On doit donc plaquer à chaud, par calandrage ou pressage, le film 6 contre le premier élément 1 pour assurer leur solidarisation l'un à l'autre.For example, the use of a
Dans l'exemple illustré, on procède à l'assemblage des différentes couches 1, 2, 3 dans le cadre d'un seul cycle de chauffage et de mise en pression.In the example illustrated, the
Bien entendu, il est envisageable d'opérer d'abord un plaquage du film 2 sur l'une des couches 1 ou 2 et ensuite d'opérer, dans un second temps, au plaquage du film 2 avec la seconde couche.Of course, it is conceivable to carry out first a plating of the
Le complexe ainsi formé est ensuite prêt à l'emploi pour servir au recouvrement d'un article composite à décorer.The complex thus formed is then ready for use to serve for covering a composite article to be decorated.
Par article composite, on entend essentiellement tout objet stratifié possédant une structure de renfort. On pense en particulier, aux skis, surfs des neiges, planches à roulette, etc.By composite article is meant essentially any laminated object having a reinforcing structure. We think in particular of skis, snowboards, skateboards, etc.
La figure 4 montre schématiquement la coupe d'un ski qui comprend un complexe obtenu selon le procédé de l'invention.Figure 4 schematically shows the section of a ski which comprises a complex obtained according to the method of the invention.
La solidarisation du complexe avec le reste de la structure du ski peut être faite dans le cadre de procédés très différents. Dans tous les cas, on procède généralement à un cycle de pressage à chaud avec la structure de renfort 4 du ski à base de résine thermofluable. Cette structure de renfort 4 peut notamment être constituée d'une nappe textile de renfort pré-imprégnée d'une résine thermodurcissable ou d'une résine thermoplastique.The connection of the complex with the rest of the ski structure can be done in very different processes. In all cases, a hot pressing cycle is generally carried out with the
On peut notamment utiliser une nappe textile de renfort à base de fibres tissées ou non tissées en verre, en carbone ou en polyaramide, imprégnée d'une résine thermodurcissable humide ou partiellement réticulée choisie dans le groupe constitué par le polyester, les époxydes, les polyuréthannes.It is in particular possible to use a reinforcing textile web based on woven or non-woven fibers of glass, carbon or polyaramide, impregnated with a wet or partially crosslinked thermosetting resin chosen from the group consisting of polyester, epoxides, polyurethanes .
En alternative, on peut utiliser une nappe textile de renfort à base de fibres tissées ou non tissées en verre ou en carbone imprégnée d'une résine thermoplastique choisie dans le groupe constitué par les polyamides, les polycarbonates, les PEI (Polyéther Imide).As an alternative, it is possible to use a reinforcing textile sheet based on woven or non-woven fibers of glass or carbon impregnated with a thermoplastic resin chosen from the group consisting of polyamides, polycarbonates, PEI (Polyether Imide).
D'une manière plus générale, la feuille de contraste 3 peut être choisie parmi le groupe constitué par l'aluminium non anodisé, la fibre sèche synthétique et le bois.More generally, the
En fonction du choix retenu, on pourra obtenir soit un rendu aux couleurs métalliques dans le cas de l'aluminium, soit un fond tramé ou tissé dans le cas de la fibre, soit encore un aspect veiné dans le cas du bois.Depending on the choice made, we can obtain either a metallic color rendering in the case of aluminum, or a woven or woven background in the case of fiber, or a veined appearance in the case of wood.
Lorsque la feuille de contraste est en fibres sèches, elle se présente avantageusement sous la forme d'une nappe (ou voile) textile non tissée ou tissée en fibres de verre , carbone, polyester, polyaramide ou autres fibres synthétiques ou naturelles, comme en coton par exemple.When the contrast sheet is made of dry fibers, it is advantageously in the form of a nonwoven or woven textile sheet (or veil) made of glass fibers, carbon, polyester, polyaramide or other synthetic or natural fibers, such as cotton for example.
Afin d'éviter toute pollution de la fibre sèche de la feuille de contraste 3 par la résine thermofluable de la structure de renfort de l'article composite à décorer, il est nécessaire d'imperméabiliser la face externe 33 à l'aide d'un film barrière 21 (figure 5).In order to avoid any pollution of the dry fiber of the
Pour cela, on profite lors du second cycle au plaquage à chaud de la couche transparente pré-sublimée 1 avec la feuille de contraste 3 au moyen du film de collage 20 pour rapporter et faire adhérer un film barrière supplémentaire 21 sur la face externe 33 ; par opposition à sa face interne 32 en contact avec le film 20. Le film de collage 20 joue un rôle important de tampon des encres de sublimation qui ont tendance à vouloir migrer naturellement dans la couche de fibre sèche 3. Le film barrière 21 quant à lui est choisi dans un matériau ayant une bonne compatibilité de collage avec la feuille de contraste 3, d'une part, et avec la résine fluable à chaud de la structure de renfort de l'article composite à décorer, d'autre part.For this, during the second cycle, advantage is taken of the hot plating of the pre-sublimed
Dans une variante, l'accostage du film barrière peut aussi se faire pendant l'assemblage final du complexe avec la structure de renfort de l'article à décorer lors du cycle ultérieur de pressage à chaud.Alternatively, the barrier film can also be docked during the final assembly of the complex with the reinforcing structure of the article to be decorated during the subsequent hot pressing cycle.
Le film barrière 21 peut être constitué dans un matériau thermoformable tel qu'en matériau ionomère, de préférence teinté dans la masse pour améliorer le contraste de la feuille 3. Le film barrière est choisi dans un matériau dont la viscosité est telle qu'il pénètre à l'intérieur des inserstices de la fibre et les bouche.The
Un autre intérêt de la fibre sèche réside dans sa capacité à éviter, tout autant, le fluage latéral du film de collage 20. Lors du cycle d'assemblage à chaud, la fibre absorbe une partie du matériau thermoplastique en fusion en raison de sa porosité.Another advantage of the dry fiber lies in its ability to prevent, as much, the lateral creep of the
A titre d'exemple, l'utilisation d'un film barrière en ionomère permet le collage d'une feuille de contraste choisie parmi les matériaux cités précédemment avec la structure de renfort à base de résine thermofluable du type époxyde.By way of example, the use of an ionomer barrier film allows the bonding of a contrast sheet chosen from the materials mentioned above with the reinforcement structure based on thermofluidable resin of the epoxy type.
La présente invention n'est pas limitée aux modes de réalisation qui ont été explicitement décrits, mais elle en inclut les diverses variantes et généralisations contenues dans le domaine des revendications ci-après.The present invention is not limited to the embodiments which have been explicitly described, but it includes the various variants and generalizations thereof contained in the field of claims below.
Claims (9)
la feuille de contraste (3) est assemblée sur la face (100) de la couche plastique (1) au moyen d'un film de collage (2) et en ce que la feuille de contraste (3) est choisie parmi le groupe constitué par l'aluminium non anodisé, la fibre sèche synthétique et le bois.
the contrast sheet (3) is assembled on the face (100) of the plastic layer (1) by means of a bonding film (2) and in that the contrast sheet (3) is chosen from the group made up by non-anodized aluminum, synthetic dry fiber and wood.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9513758 | 1995-11-15 | ||
FR9513758A FR2741008B1 (en) | 1995-11-15 | 1995-11-15 | PROCESS FOR DECORATING A COMPOSITE ARTICLE OF THE SKI, SURF OR SKATEBOARD TYPE |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0774365A1 true EP0774365A1 (en) | 1997-05-21 |
EP0774365B1 EP0774365B1 (en) | 2001-08-01 |
Family
ID=9484747
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP96115909A Expired - Lifetime EP0774365B1 (en) | 1995-11-15 | 1996-10-04 | Process for decorating composite articles such as skis, surfboards or skateboards |
Country Status (6)
Country | Link |
---|---|
US (1) | US5851331A (en) |
EP (1) | EP0774365B1 (en) |
JP (1) | JPH09193291A (en) |
AT (1) | ATE203717T1 (en) |
DE (1) | DE69614222T2 (en) |
FR (1) | FR2741008B1 (en) |
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WO1999014057A1 (en) * | 1997-09-15 | 1999-03-25 | Autotec Ag | Process for identifying objects |
EP0936080A2 (en) * | 1998-02-11 | 1999-08-18 | Fischer Gesellschaft m.b.H. | Process for decorating skis or similar |
EP0850785B1 (en) * | 1996-12-24 | 2003-04-02 | Salomon S.A. | Process for decorating a composite article such as a ski, surfboard, skateboard or cycle component |
EP1500414A1 (en) * | 2003-07-21 | 2005-01-26 | Salomon S.A. | Method for marking a gliding or rolling device with laminated structure and sport article adapted for that method for marking |
US7338066B2 (en) | 2004-01-30 | 2008-03-04 | Atomic Austria Gmbh | Method for producing a board-like gliding device, and a board-like gliding device |
FR3115493A1 (en) | 2020-10-28 | 2022-04-29 | Skis Rossignol | [TITLE] ARTICLE INCLUDING ON ITS VISIBLE FACE A DECORATED COMPOSITE MATERIAL AND ASSOCIATED METHOD |
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US6955576B2 (en) * | 2002-01-09 | 2005-10-18 | Tzong In Yeh | Slider |
FR2758730B1 (en) * | 1997-01-27 | 1999-02-26 | Rossignol Sa | SLIDING BOARD HAVING AN IMPROVED INTERNAL STRUCTURE |
AU8671398A (en) * | 1997-07-30 | 1999-02-22 | Dow Chemical Company, The | Low temperature lamination of wood |
WO2000038801A1 (en) * | 1998-12-28 | 2000-07-06 | Nidecker S.A. | Gliding board |
JP2000233598A (en) * | 1999-02-17 | 2000-08-29 | Inax Corp | Decorative molded article, and its manufacture |
US6349961B1 (en) | 1999-06-15 | 2002-02-26 | Jumbo Snowboards, Llp | Composite molded snowboard with metal edges |
US6309586B1 (en) | 1999-06-15 | 2001-10-30 | Jumbo Snowboards, Llc | Use of co-injection molding to produce composite parts including a molded snowboard with metal edges |
FR2800292B1 (en) * | 1999-10-28 | 2001-11-23 | Rossignol Sa | SLIDING BOARD AND METHOD FOR MANUFACTURING SUCH A BOARD |
US6743109B2 (en) | 2000-04-10 | 2004-06-01 | Brunswick Bowling & Billards Corporation | Decorative bowling ball and method therefor |
US7275756B2 (en) * | 2000-10-06 | 2007-10-02 | Atomic Austria Gmbh | Ski and method of manufacturing the ski |
US20020089149A1 (en) * | 2001-01-05 | 2002-07-11 | Scott Barbieri | Gliding board with varying bending properties |
EP2319594A1 (en) * | 2001-03-07 | 2011-05-11 | Crucible Intellectual Property, LLC | Gliding boards comprising amorphous alloy |
US6524419B1 (en) | 2001-11-30 | 2003-02-25 | Brunswick Bowling & Billiards Corporation | Method and apparatus for making and/or decorating bowling balls and the like |
WO2003066322A1 (en) * | 2002-02-05 | 2003-08-14 | Wham-O, Inc. | Laminate inlay process for sports boards |
JP2005529691A (en) * | 2002-06-13 | 2005-10-06 | ピビット,リミティド ライアビリティー カンパニー | Safety balance device |
DE10236959B4 (en) * | 2002-08-13 | 2004-10-07 | Leonhard Kurz Gmbh & Co. Kg | Multi-layer film for the construction of skis |
EP1588837B1 (en) * | 2003-01-10 | 2013-05-29 | Hasepro, Inc. | Reinforcing fiber sheet, dress-up sheet, and method of manufacturing a reinforcing fiber sheet |
JP4469334B2 (en) * | 2003-01-10 | 2010-05-26 | 株式会社ハセ・プロ | Reinforcing fiber sheet |
FR2851174B1 (en) * | 2003-02-18 | 2005-03-25 | Rossignol Sa | OUTDOOR SLIDING SNOWBOARD COMPRISING A TRANSPARENT PROTECTIVE FILM AND METHOD OF MAKING SAME |
US20050206130A1 (en) * | 2004-03-16 | 2005-09-22 | Keith Parten | Recreation board with high-definition graphics |
FR2878447B1 (en) | 2004-12-01 | 2007-02-23 | Salomon Sa | METHOD FOR DECORATING A SLIDING OR SLIDING BOARD AND A SLIDING OR ROLLING BOARD OBTAINED BY SAID DECORATION METHOD |
EP1724098A1 (en) | 2005-05-20 | 2006-11-22 | Carbo Tech Composites GmbH | Process for the production of a laminated composite product and a composite product made by the lamination process |
US7416401B2 (en) * | 2005-06-13 | 2008-08-26 | The Boeing Company | Lightweight composite fairing bar and method for manufacturing the same |
US20080248261A1 (en) * | 2007-04-05 | 2008-10-09 | Bonnett Robert A | Printed article |
AT11519U1 (en) * | 2010-01-27 | 2010-12-15 | Atomic Austria Gmbh | METHOD FOR PRODUCING AN OUTER LIMITING ELEMENT FOR A SLIDING BODY AND METHOD FOR PRODUCING A SLIDING BODY THEREFORE EQUIPPED |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0850785B1 (en) * | 1996-12-24 | 2003-04-02 | Salomon S.A. | Process for decorating a composite article such as a ski, surfboard, skateboard or cycle component |
WO1999014057A1 (en) * | 1997-09-15 | 1999-03-25 | Autotec Ag | Process for identifying objects |
US6315855B1 (en) | 1997-09-15 | 2001-11-13 | Autotec Ag | Process for identifying objects |
EP0936080A2 (en) * | 1998-02-11 | 1999-08-18 | Fischer Gesellschaft m.b.H. | Process for decorating skis or similar |
EP0936080A3 (en) * | 1998-02-11 | 2000-07-05 | Fischer Gesellschaft m.b.H. | Process for decorating skis or similar |
EP1500414A1 (en) * | 2003-07-21 | 2005-01-26 | Salomon S.A. | Method for marking a gliding or rolling device with laminated structure and sport article adapted for that method for marking |
FR2857880A1 (en) * | 2003-07-21 | 2005-01-28 | Salomon Sa | METHOD FOR MARKING A LAMINATED STRUCTURE-RUNNING OR SLIDING MACHINE AND SPORT MACHINE SUITABLE FOR THE MARKING METHOD |
US7338066B2 (en) | 2004-01-30 | 2008-03-04 | Atomic Austria Gmbh | Method for producing a board-like gliding device, and a board-like gliding device |
FR3115493A1 (en) | 2020-10-28 | 2022-04-29 | Skis Rossignol | [TITLE] ARTICLE INCLUDING ON ITS VISIBLE FACE A DECORATED COMPOSITE MATERIAL AND ASSOCIATED METHOD |
EP3991982A1 (en) | 2020-10-28 | 2022-05-04 | Skis Rossignol | Process for decorating a sliding board and sliding board including a decorated composite material on its visible surface |
US11840106B2 (en) | 2020-10-28 | 2023-12-12 | Skis Rossignol | Sliding board including on its visible face a decorated composite material and associated method |
Also Published As
Publication number | Publication date |
---|---|
FR2741008A1 (en) | 1997-05-16 |
US5851331A (en) | 1998-12-22 |
EP0774365B1 (en) | 2001-08-01 |
DE69614222T2 (en) | 2002-06-13 |
DE69614222D1 (en) | 2001-09-06 |
ATE203717T1 (en) | 2001-08-15 |
FR2741008B1 (en) | 1998-01-30 |
JPH09193291A (en) | 1997-07-29 |
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