EP1143029A1 - Method for manufacturing a body featuring very high mechanical properties, forming by drawing from a rolled steel sheet, in particular hot rolled and coated sheet - Google Patents

Method for manufacturing a body featuring very high mechanical properties, forming by drawing from a rolled steel sheet, in particular hot rolled and coated sheet Download PDF

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Publication number
EP1143029A1
EP1143029A1 EP01400861A EP01400861A EP1143029A1 EP 1143029 A1 EP1143029 A1 EP 1143029A1 EP 01400861 A EP01400861 A EP 01400861A EP 01400861 A EP01400861 A EP 01400861A EP 1143029 A1 EP1143029 A1 EP 1143029A1
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EP
European Patent Office
Prior art keywords
sheet
steel
zinc
stamping
metal
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
EP01400861A
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German (de)
French (fr)
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EP1143029B1 (en
Inventor
Ronald Kefferstein
Xavier Jartoux
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.)
ArcelorMittal France SA
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USINOR SA
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Application filed by USINOR SA filed Critical USINOR SA
Priority to DE20122563U priority Critical patent/DE20122563U1/en
Priority to EP10006299.1A priority patent/EP2224034B1/en
Priority to EP06002618.4A priority patent/EP1672088B2/en
Publication of EP1143029A1 publication Critical patent/EP1143029A1/en
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Publication of EP1143029B1 publication Critical patent/EP1143029B1/en
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    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0278—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips involving a particular surface treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D22/00—Shaping without cutting, by stamping, spinning, or deep-drawing
    • B21D22/20—Deep-drawing
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/06—Zinc or cadmium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/26—After-treatment
    • C23C2/28—Thermal after-treatment, e.g. treatment in oil bath
    • C23C2/29—Cooling or quenching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
    • C23C2/36—Elongated material
    • C23C2/40—Plates; Strips
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/62—Quenching devices
    • C21D1/673—Quenching devices for die quenching

Definitions

  • the invention relates to a method for producing a part with very high mechanical characteristics, shaped by stamping, from a strip of rolled steel sheet, in particular hot rolled and coated with a metal or a metal alloy providing surface and steel protection.
  • the heat treatment must be carried out under a controlled atmosphere in order to avoid any decarburization and oxidation of the steel.
  • the scale by its abrasive power, damages the forming tools, which reduces the quality of the parts obtained from the dimensional and aesthetic point of view or requires frequent and costly repairs. of tools.
  • the parts thus obtained must receive an expensive post-treatment, the application of which is difficult, if not impossible, in particular in the case of parts comprising recesses.
  • the post-coatings of steels with very high mechanical characteristics also have the disadvantage of creating risks of embrittlement by hydrogen in electro-galvanizing techniques or of modifying the mechanical properties of these steels in techniques of galvanizing by dipping of previously formed parts.
  • the object of the invention is to provide users with laminated steel sheets from 0.2 mm to around 4 mm thick, coated in particular after hot rolling, and having to undergo a shaping, either hot or cold followed by a treatment thermal, as well as a method of producing a part by hot forming, from these coated steel sheets, the temperature rise being ensured without decarburization sheet steel, without oxidation of the surface of said sheet, before, during and after hot forming and or heat treatment.
  • the invention also relates to the use of a strip of laminated steel sheet and in particular hot rolled and coated with a metal or a metal alloy ensuring protection of the surface and the steel of the sheet in forming by especially hot stamping of parts, the parts having high mechanical characteristics in hardness and high hardness characteristics in surface as well as very good abrasion resistance.
  • FIG. 1 is a block diagram of one form of the invention.
  • FIG. 2 is a block diagram of another form of the invention.
  • Figures 3a and 3b are sectional photographs of part of a room, having a zinc coating produced according to the invention, before and after treatment thermal.
  • Figures 4a and 4b are sectional photographs of part of a room, having a zinc aluminum coating produced according to the invention, before and after heat treatment.
  • the method according to the invention as presented in the diagram of FIG. 1, consists, from a sheet of steel for heat treatment and or hot forming especially hot rolled and coated with zinc or a zinc-based alloy, production of a hot-formed part using a tool such as a press stamping.
  • the zinc or zinc alloy coating is chosen so as to generate a protection against corrosion of the base sheet, in coil.
  • the coating forms a layer which combines with the steel of the strip and at this time exhibits an outfit mechanical avoiding the melting of coating metal.
  • the compound formed has a high resistance to corrosion, abrasion, wear and fatigue.
  • the coating does not modify the formability properties of steel and thus allows great variety of cold and hot shaping.
  • the strip After hot rolling, the strip can be pickled and cold rolled before to be clothed. In the case where the sheet is cold rolled, it can be annealed before to be clothed.
  • the laminated sheet can be coated, for example, with zinc, or zinc alloys aluminum.
  • the sheet can be stamped at cold to obtain the part.
  • the part obtained is then subjected to a treatment.
  • a base steel having a tensile strength Rm of around 500 MPa will allow obtaining heat treated parts having steel with Rm resistance greater than 1500 MPa.
  • the sheet is subjected to a temperature rise preferably between 700 ° C and 1200 ° C in an oven with an atmosphere no longer requiring control, made of the barrier to oxidation formed by the coating.
  • a temperature rise preferably between 700 ° C and 1200 ° C in an oven with an atmosphere no longer requiring control, made of the barrier to oxidation formed by the coating.
  • the zinc-based coating turns into an alloy layer in surface comprising different phases depending on the temperature treatment and with a high hardness that can exceed 600 HV 100g.
  • the sheets supplied coated have a high resistance to corrosion during temperature rises, shaping, heat treatments, and when using finished formed parts.
  • the presence of the coating during heat treatments or forming hot prevents decarburization of the base steel. That to an undeniable advantage in the case of hot shaping for example in a stamping press.
  • the intermetallic alloy formed avoids, the formation scale, wear of tools by scale, and thus allows an elongation of the average life of said tools.
  • the intermetallic alloy formed at hot has a high temperature lubricant function.
  • the protective effect against decarburization of the intermetallic alloy allows the use of high furnace temperature exceeding 900 ° C with an uncontrolled atmosphere, even for heating times of several minutes.
  • the parts obtained Due to the characteristics of the coating after temperature rise, the parts obtained have increased resistance to fatigue, wear, abrasion and corrosion, including on edge due to the galvanic behavior of zinc with steel.
  • the coating is weldable before and after temperature rise.
  • the sheet steel ensures, by cooling quenching effect, high mechanical characteristics of the part obtained after shaping, the coating transformed into a hot intermetallic alloy ensuring for its part, made of its qualities of lubricant and resistance to friction, an improvement of the shaping, in particular, in the field of hot stamping.
  • Example 1 zinc coating on steel.
  • a part is made from 1mm thick cold-rolled steel sheet and continuously double-sided galvanized, with a coating thickness of 10 ⁇ m about.
  • the sheet is austenitized at 950 ° C. before forming and quenching in the tool, the coating providing a role of lubricant during shaping, in addition to its protection functions against cold, hot corrosion and decarburization.
  • the alloy coating does not interfere with the extraction of heat by the tool and can promote it. After forming and quenching, it is no longer necessary to strip the part or to protect it, the base coating providing protection throughout the process.
  • the part produced is a matt gray appearance without sagging or bubbles, without flaking or cracks, and not presenting no scale on the edge, in section.
  • Microscope observations scanning electronics show on the surface and in section, that the coating keeps a homogeneous structure and texture and that the Fe-Zn alloy manifests in less than 5 minutes at 950 ° C.
  • the coating comprises as shown in a comparative manner on the Figures 3a and 3b respectively representing, in section, the coating before and after heat treatment, a Zn diffusion interface, with a thickness between 5 and 10 ⁇ m, is a layer formed by Zn-Fe alloy nodules in a matrix zinc, layer with a thickness between 10 and 15 ⁇ m.
  • Table 1 below shows the loss of mass by corrosion after 500 and 1000 hours of salt spray, for an uncoated reference steel, for a galvanized reference steel without heat treatment, and a steel according to two forms of the invention.
  • Mass losses in g / m 2 After 500 hours Mass losses in g / m 2 After 1000 hours
  • the coating after heat treatment resists well in salt spray.
  • this surface composed of zinc and iron, can phosphating in conventional surface treatment baths of the phosphating type trication. Corrosion tests carried out after phosphating and cataphoresis painting show excellent results.
  • the zinc-iron alloy layer also provides protection galvanic of the cathodic protection type wafers.
  • Example 2 coating of aluminum zinc on steel.
  • a 10 ⁇ m coating is applied to a sheet of approximately 1mm.
  • This coating is composed of 50 to 55% aluminum and 45 to 50% zinc with possibly a small amount of silicon.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Coating With Molten Metal (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Shaping Metal By Deep-Drawing, Or The Like (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Forging (AREA)
  • Heat Treatment Of Articles (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Laminated Bodies (AREA)
  • Pressure Welding/Diffusion-Bonding (AREA)

Abstract

A method for the production of a component with very high mechanical characteristics, by pressing a hot rolled steel strip coated with a protective metal or alloy, consists of cutting the strip to form a blank, pressing the blank to form the component, the production, before or after pressing, of an allied intermetallic compound at the surface acting as a lubricant and removing the surplus strip needed by the pressing operation. An Independent claim is included for the utilisation of a hot rolled steel strip coated with a protective metal or alloy in pressing operations.

Description

L'invention concerne un procédé de réalisation d'une pièce à très hautes caractéristiques mécaniques, mise en forme par emboutissage, à partir d'une bande de tôle d'acier laminée et notamment laminée à chaud et revêtue d'un métal ou d'un alliage métallique assurant une protection de la surface et de l'acier.The invention relates to a method for producing a part with very high mechanical characteristics, shaped by stamping, from a strip of rolled steel sheet, in particular hot rolled and coated with a metal or a metal alloy providing surface and steel protection.

Les tôles en acier devant subir un formage à haute température et ou un traitement thermique ne sont pas livrées revêtues pour des considérations de tenue du revêtement lors du traitement thermique, le traitement thermique des aciers se faisant généralement à des températures relativement élevées bien supérieures à 700°C. En effet, un revêtement de zinc déposé sur une surface métallique a été considéré jusqu'à présent comme pouvant fondre, s'écouler, encrasser les outils de formage à chaud, lors de chauffage, à des températures supérieures à la température de fusion du zinc, et se dégrader lors d'un refroidissement rapide.
Le revêtement est donc effectué sur pièce finie ce qui nécessite un nettoyage soigné des surfaces et des parties creuses. Ce nettoyage requiert l'utilisation d'acides et ou de bases dont le recyclage et le stockage sont une charge financière importante et présentent des risques pour les opérateurs et pour l'environnement. De plus, le traitement thermique doit être effectué sous atmosphère contrôlée afin d'éviter toute décarburation et oxydation de l'acier. Ensuite, dans le cas du formage à chaud, la calamine, de par son pouvoir abrasif, endommage les outils de mise en forme, ce qui diminue la qualité des pièces obtenues du point de vue dimensionnel et esthétique ou oblige à de fréquentes et coûteuses réparations d'outils. Enfin, pour augmenter leur résistance à la corrosion, les pièces ainsi obtenues doivent recevoir un post traitement coûteux dont l'application est difficile, voire impossible, en particulier dans le cas de pièces comportant des creux. Les post-revêtements des aciers à très hautes caractéristiques mécaniques ont également comme inconvénient de créer des risques de fragilisation par l'hydrogène dans les techniques d'électro-zingage ou de modifier les propriétés mécaniques de ces aciers dans des techniques de galvanisation au trempé des pièces préalablement formées.Steel sheets having to undergo high temperature forming and or heat treatment are not supplied coated for reasons of resistance of the coating during heat treatment, the heat treatment of steels generally being carried out at relatively high temperatures well above 700 ° C. Indeed, a coating of zinc deposited on a metal surface has been considered until now as being able to melt, flow, foul the hot forming tools, during heating, at temperatures higher than the melting temperature of the zinc. , and degrade during rapid cooling.
The coating is therefore carried out on a finished part, which requires careful cleaning of the surfaces and of the hollow parts. This cleaning requires the use of acids and or bases, the recycling and storage of which are a significant financial burden and present risks for operators and the environment. In addition, the heat treatment must be carried out under a controlled atmosphere in order to avoid any decarburization and oxidation of the steel. Then, in the case of hot forming, the scale, by its abrasive power, damages the forming tools, which reduces the quality of the parts obtained from the dimensional and aesthetic point of view or requires frequent and costly repairs. of tools. Finally, to increase their resistance to corrosion, the parts thus obtained must receive an expensive post-treatment, the application of which is difficult, if not impossible, in particular in the case of parts comprising recesses. The post-coatings of steels with very high mechanical characteristics also have the disadvantage of creating risks of embrittlement by hydrogen in electro-galvanizing techniques or of modifying the mechanical properties of these steels in techniques of galvanizing by dipping of previously formed parts.

Le but de l'invention est de proposer aux utilisateurs, des tôles d'acier laminées de 0,2 mm à environ 4 mm d'épaisseur, revêtues notamment après laminage à chaud, et devant subir une mise en forme, soit à chaud, soit à froid suivie d'un traitement thermique, ainsi qu'un procédé de réalisation de pièce par formage à chaud, à partir de ces tôles d'acier revêtues, l'élévation de température étant assurée sans décarburation de l'acier de la tôle, sans oxydation de la surface de ladite tôle, avant, pendant et après la mise en forme à chaud et ou le traitement thermique.The object of the invention is to provide users with laminated steel sheets from 0.2 mm to around 4 mm thick, coated in particular after hot rolling, and having to undergo a shaping, either hot or cold followed by a treatment thermal, as well as a method of producing a part by hot forming, from these coated steel sheets, the temperature rise being ensured without decarburization sheet steel, without oxidation of the surface of said sheet, before, during and after hot forming and or heat treatment.

L'invention a pour objet un procédé de réalisation d'une pièce à très hautes caractéristiques mécaniques, mise en forme par emboutissage, à partir d'une bande de tôle d'acier laminée, notamment laminée à chaud et revêtue d'un métal ou d'un alliage métallique assurant une protection de la surface et de l'acier, caractérisée en ce que :

  • on découpe la tôle pour l'obtention d'un flan de tôle,
  • on effectue un emboutissage, à partir du flan de tôle pour obtenir la pièce,
  • on réalise, avant ou après emboutissage, un composé allié intermétallique, en surface, assurant une protection contre la corrosion, contre la décarburation de l'acier, le composé intermétallique pouvant assurer une fonction de lubrification,
  • on retire par découpage, les excédents de tôle nécessaires à l'opération d'emboutissage.
The subject of the invention is a process for producing a part with very high mechanical characteristics, shaped by stamping, from a strip of rolled steel sheet, in particular hot rolled and coated with a metal or of a metal alloy ensuring protection of the surface and of the steel, characterized in that:
  • the sheet is cut to obtain a sheet blank,
  • stamping is carried out from the sheet blank to obtain the part,
  • before or after drawing, an alloyed intermetallic compound is produced on the surface, providing protection against corrosion, against decarburization of steel, the intermetallic compound being able to provide a lubrication function,
  • the excess sheet metal necessary for the stamping operation is removed by cutting.

Dans une forme préférentielle de l'invention,

  • on découpe la tôle pour l'obtention d'un flan de tôle,
  • on soumet le flan de tôle revêtue à une élévation en température dans le but de former une pièce à chaud,
  • on réalise, de ce fait un composé allié intermétallique, en surface, assurant une protection contre la corrosion, contre la décarburation de l'acier, le composé intermétallique pouvant assurer une fonction de lubrification,
  • on effectue la mise en forme du flan de tôle, par emboutissage,
  • on refroidit la pièce formée pour conférer des caractéristiques mécaniques de dureté élevées de l'acier et une dureté superficielle élevée du revêtement,
  • on retire par découpage, les excédents de tôle nécessaires à l'opération d'emboutissage.
In a preferred form of the invention,
  • the sheet is cut to obtain a sheet blank,
  • the coated sheet metal blank is subjected to a rise in temperature in order to form a hot part,
  • this produces an alloyed intermetallic compound, on the surface, providing protection against corrosion, against decarburization of steel, the intermetallic compound being able to provide a lubrication function,
  • the sheet blank is shaped, by stamping,
  • the formed part is cooled to give mechanical characteristics of high hardness of the steel and a high surface hardness of the coating,
  • the excess sheet metal necessary for the stamping operation is removed by cutting.

Les autres caractéristiques de l'invention sont :

  • le métal ou l'alliage métallique du revêtement est du zinc ou un alliage à base de zinc d'une épaisseur comprise entre 5 µm et 30 µm.
  • l'alliage intermétallique est un composé à base de zinc-fer ou à base de zinc-fer-aluminium.
  • la tôle revêtue est soumise à une élévation de température supérieure à 700°C avant la mise en forme et ou le traitement thermique.
  • la pièce obtenue notamment par emboutissage est refroidie pour subir une trempe, à une vitesse supérieure à la vitesse critique de trempe.
The other characteristics of the invention are:
  • the metal or metal alloy of the coating is zinc or a zinc-based alloy with a thickness of between 5 μm and 30 μm.
  • the intermetallic alloy is a compound based on zinc-iron or based on zinc-iron-aluminum.
  • the coated sheet is subjected to a temperature rise above 700 ° C. before forming and or heat treatment.
  • the part obtained in particular by stamping is cooled to undergo quenching, at a speed greater than the critical quenching speed.

L'invention concerne aussi l'utilisation d'une bande de tôle d'acier laminée et notamment laminée à chaud et revêtue d'un métal ou d'un alliage métallique assurant une protection de la surface et de l'acier de la tôle dans la mise en forme par emboutissage notamment à chaud de pièces, les pièces ayant de hautes caractéristiques mécaniques en dureté et de hautes caractéristiques de dureté en surface ainsi qu'une très bonne tenue à l'abrasion.The invention also relates to the use of a strip of laminated steel sheet and in particular hot rolled and coated with a metal or a metal alloy ensuring protection of the surface and the steel of the sheet in forming by especially hot stamping of parts, the parts having high mechanical characteristics in hardness and high hardness characteristics in surface as well as very good abrasion resistance.

La description qui suit et les figures annexées feront bien comprendre l'invention.The following description and the appended figures will make the invention easier to understand.

La figure 1 est un schéma de principe d'une forme de l'invention.Figure 1 is a block diagram of one form of the invention.

La figure 2 est un schéma de principe d'une autre forme de l'invention.Figure 2 is a block diagram of another form of the invention.

Les figures 3a et 3b sont des photographies, en coupe, d'une partie de pièce, présentant un revêtement zinc réalisé selon l'invention, avant et après traitement thermique.Figures 3a and 3b are sectional photographs of part of a room, having a zinc coating produced according to the invention, before and after treatment thermal.

Les figures 4a et 4b sont des photographies, en coupe, d'une partie de pièce, présentant un revêtement zinc aluminium réalisé selon l'invention, avant et après traitement thermique.Figures 4a and 4b are sectional photographs of part of a room, having a zinc aluminum coating produced according to the invention, before and after heat treatment.

Le procédé selon l'invention comme présenté sur le schéma de la figure 1, consiste, à partir d'une tôle d'un acier pour traitement thermique et ou formage à chaud notamment laminé à chaud et revêtu de zinc ou d'un alliage à base de zinc, en la réalisation de pièce mise en forme à chaud au moyen d'outil comme une presse d'emboutissage.The method according to the invention as presented in the diagram of FIG. 1, consists, from a sheet of steel for heat treatment and or hot forming especially hot rolled and coated with zinc or a zinc-based alloy, production of a hot-formed part using a tool such as a press stamping.

Le revêtement de zinc ou d'alliage de zinc est choisi de manière à générer une protection contre la corrosion de la tôle de base, en bobine.The zinc or zinc alloy coating is chosen so as to generate a protection against corrosion of the base sheet, in coil.

Contrairement aux idées reçues, lors d'un traitement thermique ou d'une élévation de température pour la mise en forme à chaud, le revêtement forme une couche qui s'allie avec l'acier de la bande et présente à ce moment une tenue mécanique évitant la fusion de métal de revêtement. Le composé formé présente une grande résistance à la corrosion, à l'abrasion, à l'usure et à la fatigue. Le revêtement ne modifie pas les propriétés de formabilité de l'acier et autorise ainsi une grande variété de mise en forme à froid et à chaud.Contrary to popular belief, during a heat treatment or temperature rise for hot forming, the coating forms a layer which combines with the steel of the strip and at this time exhibits an outfit mechanical avoiding the melting of coating metal. The compound formed has a high resistance to corrosion, abrasion, wear and fatigue. The coating does not modify the formability properties of steel and thus allows great variety of cold and hot shaping.

De plus l'utilisation du zinc ou d'un alliage de zinc génère une protection galvanique des tranches lorsque le flan de tôle ou la pièce présente des découpes. In addition the use of zinc or a zinc alloy generates protection galvanic slices when the sheet metal blank or the part has cuts.

Après laminage à chaud, la bande peut être décapée et laminée à froid avant d'être revêtue. Dans le cas ou la tôle est laminée à froid, celle ci peut être recuite avant d'être revêtue.After hot rolling, the strip can be pickled and cold rolled before to be clothed. In the case where the sheet is cold rolled, it can be annealed before to be clothed.

On peut revêtir la tôle laminée, par exemple, avec du zinc, ou des alliages zinc aluminium.The laminated sheet can be coated, for example, with zinc, or zinc alloys aluminum.

Comme représenté sur le schéma de la figure 2, la tôle peut être emboutie à froid pour l'obtention de la pièce. La pièce obtenue est ensuite soumise à un traitement thermique pour lui conférer des caractéristiques mécaniques élevées. Par exemple, un acier de base ayant une résistance à la rupture Rm d'environ 500 MPa permettra d'obtention de pièces traitées thermiquement ayant un acier avec une résistance Rm supérieure à 1500 MPa.As shown in the diagram in Figure 2, the sheet can be stamped at cold to obtain the part. The part obtained is then subjected to a treatment. thermal to give it high mechanical properties. For example, a base steel having a tensile strength Rm of around 500 MPa will allow obtaining heat treated parts having steel with Rm resistance greater than 1500 MPa.

Pour la mise en forme ou pour le traitement thermique de la pièce, la tôle est soumise à une élévation de température comprise de préférence entre 700°C et 1200°C dans un four comportant une atmosphère ne nécessitant plus de contrôle, du fait de la barrière à l'oxydation formée par le revêtement. Lors de l'élévation de la température, le revêtement à base de zinc se transforme en une couche alliée en surface comportant différentes phases dépendant du traitement en température et présentant une grande dureté pouvant dépasser 600 HV 100g.For the shaping or for the heat treatment of the part, the sheet is subjected to a temperature rise preferably between 700 ° C and 1200 ° C in an oven with an atmosphere no longer requiring control, made of the barrier to oxidation formed by the coating. When raising the temperature, the zinc-based coating turns into an alloy layer in surface comprising different phases depending on the temperature treatment and with a high hardness that can exceed 600 HV 100g.

Dans le procédé de l'invention, on peut utiliser des tôles dont l'épaisseur est comprise entre 0,2 mm et 4 mm, ayant de bonnes propriétés de mise en forme ainsi qu'une bonne résistance à la corrosion.In the process of the invention, it is possible to use sheets whose thickness is between 0.2 mm and 4 mm, having good shaping properties as well good resistance to corrosion.

Les tôles livrées revêtues, présentent une résistance importante à la corrosion pendant les élévations de température, la mise en forme, les traitements thermiques, et lors de l'utilisation des pièces formées finies.The sheets supplied coated, have a high resistance to corrosion during temperature rises, shaping, heat treatments, and when using finished formed parts.

La présence du revêtement lors de traitements thermiques ou de formages à chaud permet d'éviter en plus de la corrosion, la décarburation de l'acier de base. Cela à un avantage indéniable dans le cas d'une mise en forme à chaud par exemple dans une presse d'emboutissage. En effet, l'alliage intermétallique formé évite, la formation de la calamine, l'usure des outils par la calamine, et permet de ce fait, un allongement de la vie moyenne desdits outils. Il a été remarqué que l'alliage intermétallique formé à chaud, a une fonction de lubrifiant à haute température. De plus, l'effet de protection contre la décarburation de l'alliage intermétallique permet l'usage de four haute température dépassant 900°C ayant une atmosphère non contrôlée, et cela, même pour des temps de chauffe de plusieurs minutes. The presence of the coating during heat treatments or forming hot, in addition to corrosion, prevents decarburization of the base steel. That to an undeniable advantage in the case of hot shaping for example in a stamping press. Indeed, the intermetallic alloy formed avoids, the formation scale, wear of tools by scale, and thus allows an elongation of the average life of said tools. It has been noted that the intermetallic alloy formed at hot, has a high temperature lubricant function. In addition, the protective effect against decarburization of the intermetallic alloy allows the use of high furnace temperature exceeding 900 ° C with an uncontrolled atmosphere, even for heating times of several minutes.

En sortie de four, il n'est plus nécessaire de décaper la pièce obtenue, d'où une économie du fait de la suppression du bain de décapage des pièces finies.At the exit of the oven, it is no longer necessary to strip the part obtained, resulting in a savings due to the elimination of the pickling bath for finished parts.

De par les caractéristiques du revêtement après élévation de température, les pièces obtenues ont une résistance accrue à la fatigue, à l'usure, à l'abrasion et à la corrosion, y compris sur tranche du fait du comportement galvanique du zinc avec l'acier. De plus, le revêtement est soudable avant et après élévation de température.Due to the characteristics of the coating after temperature rise, the parts obtained have increased resistance to fatigue, wear, abrasion and corrosion, including on edge due to the galvanic behavior of zinc with steel. In addition, the coating is weldable before and after temperature rise.

L'acier de la tôle assure, par effet de trempe au refroidissement, des caractéristiques mécaniques élevées de la pièce obtenue après mise en forme, le revêtement transformé en un alliage intermétallique à chaud assurant pour sa part, du fait de ses qualités de lubrifiant et de résistance aux frottements, une amélioration de la mise en forme, notamment, dans le domaine de l'emboutissage à chaud.The sheet steel ensures, by cooling quenching effect, high mechanical characteristics of the part obtained after shaping, the coating transformed into a hot intermetallic alloy ensuring for its part, made of its qualities of lubricant and resistance to friction, an improvement of the shaping, in particular, in the field of hot stamping.

Exemple 1 : revêtement de zinc sur acier.Example 1: zinc coating on steel.

Dans un exemple de réalisation, on utilise une bande de tôle laminée à chaud en acier de composition pondérale suivante :

  • carbone : 0,15% à 0,25%,
  • manganèse : 0,8% à 1,5%,
  • silicium : 0,1% à 0,35%,
  • chrome : 0,01% à 0,2%,
  • titane : moins de 0,1%,
  • aluminium : moins de 0,1%,
  • phosphore : moins de 0,05%,
  • soufre : moins de 0,03%,
  • bore : 0,0005% à 0,01%.
    • In an exemplary embodiment, a strip of hot-rolled steel sheet of the following composition by weight is used:
  • carbon: 0.15% to 0.25%,
  • manganese: 0.8% to 1.5%,
  • silicon: 0.1% to 0.35%,
  • chromium: 0.01% to 0.2%,
  • titanium: less than 0.1%,
  • aluminum: less than 0.1%,
  • phosphorus: less than 0.05%,
  • sulfur: less than 0.03%,
  • boron: 0.0005% to 0.01%.

    • On réalise une pièce à partir de la tôle d'acier laminé à froid de 1mm d'épaisseur et galvanisée en continu double face, avec une épaisseur de revêtement de 10 µm environ. On austénitise la tôle à 950°C avant formage et trempe dans l'outil, le revêtement assurant un rôle de lubrifiant lors de la mise en forme, en plus de ses fonctions de protection contre la corrosion à froid, à chaud et contre la décarburation. Lors de la trempe, le revêtement allié ne gène pas l'extraction de la chaleur par l'outil et peut la favoriser. Après formage et trempe, il n'est plus nécessaire de décaper la pièce ou de la protéger, le revêtement de base assurant la protection tout au long du procédé.A part is made from 1mm thick cold-rolled steel sheet and continuously double-sided galvanized, with a coating thickness of 10 µm about. The sheet is austenitized at 950 ° C. before forming and quenching in the tool, the coating providing a role of lubricant during shaping, in addition to its protection functions against cold, hot corrosion and decarburization. During hardening, the alloy coating does not interfere with the extraction of heat by the tool and can promote it. After forming and quenching, it is no longer necessary to strip the part or to protect it, the base coating providing protection throughout the process.

    Après mise en forme et de ce fait, traitement thermique, la pièce réalisée est d'un aspect gris mat sans coulure ni bulle, sans écaillage ou fissures, et ne présentant pas de calamine sur la tranche, en coupe. Des observations au microscope électronique à balayage montrent en surface et en coupe, que le revêtement garde une structure et une texture homogènes et que l'alliation Fe-Zn se manifeste en moins de 5 minutes à 950°C.After shaping and therefore heat treatment, the part produced is a matt gray appearance without sagging or bubbles, without flaking or cracks, and not presenting no scale on the edge, in section. Microscope observations scanning electronics show on the surface and in section, that the coating keeps a homogeneous structure and texture and that the Fe-Zn alloy manifests in less than 5 minutes at 950 ° C.

    Le revêtement comprend comme représenté de manière comparative sur les figures 3a et 3b représentant respectivement, en coupe, le revêtement avant et après traitement thermique, une interface de diffusion du Zn, d'une épaisseur comprise entre 5 et 10 µm, est une couche formée par des nodules d'alliage Zn-Fe dans une matrice de zinc, couche d'une épaisseur comprise entre 10 et 15 µm.The coating comprises as shown in a comparative manner on the Figures 3a and 3b respectively representing, in section, the coating before and after heat treatment, a Zn diffusion interface, with a thickness between 5 and 10 µm, is a layer formed by Zn-Fe alloy nodules in a matrix zinc, layer with a thickness between 10 and 15 µm.

    Des essais de corrosion en humidité et température suivant la norme DIN 50 017 montrent que le revêtement selon l'invention assure une excellente protection contre la corrosion après 30 cycles, les surfaces des pièces gardant leur aspect gris.Corrosion tests in humidity and temperature according to DIN 50 017 show that the coating according to the invention provides excellent protection against corrosion after 30 cycles, the surfaces of the parts retaining their gray appearance.

    Le tableau 1 suivant présente la perte de masse par corrosion après 500 et 1000 heures de brouillard salin, pour un acier de référence non revêtu, pour un acier de référence galvanisé sans traitement thermique, et un acier selon deux formes de l'invention. Pertes de masse en g/m2 Après 500 heures Pertes de masse en g/m2 Après 1000 heures Acier de référence 450 g/m2 1230 g/m2 Acier galvanisé de référence 80 g/m2 140 g/m2 Acier revêtu Zn après traitement thermique 32 g/m2 82 g/m2 Acier revêtu Zn-AI après traitement thermique 22 g/m2 50 g/m2 Table 1 below shows the loss of mass by corrosion after 500 and 1000 hours of salt spray, for an uncoated reference steel, for a galvanized reference steel without heat treatment, and a steel according to two forms of the invention. Mass losses in g / m 2 After 500 hours Mass losses in g / m 2 After 1000 hours Reference steel 450 g / m 2 1230 g / m 2 Reference galvanized steel 80 g / m 2 140 g / m 2 Zn coated steel after heat treatment 32 g / m 2 82 g / m 2 Zn-AI coated steel after heat treatment 22 g / m 2 50 g / m 2

    Comme on peut le remarquer, le revêtement après traitement thermique résiste bien au brouillard salin. De plus cette surface, composée de zinc et de fer peut se phosphater dans des bains classiques de traitement de surface du type phosphatation trication. Les essais de corrosion réalisés après phosphatation et peinture cataphorèse montrent d'excellents résultats. La couche alliée zinc fer assure de plus une protection galvanique des tranches du type protection cathodique.As can be seen, the coating after heat treatment resists well in salt spray. In addition, this surface, composed of zinc and iron, can phosphating in conventional surface treatment baths of the phosphating type trication. Corrosion tests carried out after phosphating and cataphoresis painting show excellent results. The zinc-iron alloy layer also provides protection galvanic of the cathodic protection type wafers.

    Exemple 2 : revêtement de zinc aluminium sur acier.Example 2: coating of aluminum zinc on steel.

    Un revêtement de 10 µm est appliqué sur une tôle de 1mm environ. Ce revêtement est composé de 50 à 55% d'aluminium et de 45 à 50% de zinc avec éventuellement une petite quantité de silicium. A 10 µm coating is applied to a sheet of approximately 1mm. This coating is composed of 50 to 55% aluminum and 45 to 50% zinc with possibly a small amount of silicon.

    L'aspect de ce revêtement en coupe, après formage à chaud est présenté sur les figures 4a et 4b.The appearance of this coating in section, after hot forming is presented on Figures 4a and 4b.

    Lors du formage à chaud, le zinc, l'aluminium, et le fer s'allient pour former un revêtement de zinc-aluminium-fer homogène et adhérent. Les tests de corrosion montrent que cette couche alliée assure une très bonne protection contre la corrosion.During hot forming, zinc, aluminum, and iron combine to form a homogeneous and adherent zinc-aluminum-iron coating. Corrosion tests show that this alloy layer provides very good protection against corrosion.

    Claims (7)

    Procédé de réalisation d'une pièce à très hautes caractéristiques mécaniques, mise en forme par emboutissage, à partir d'une bande de tôle d'acier laminée, notamment laminée à chaud et revêtue d'un métal ou d'un alliage métallique assurant une protection de la surface et de l'acier, caractérisée en ce que : on découpe la tôle pour l'obtention d'un flan de tôle, on effectue un emboutissage, à partir du flan de tôle pour obtenir la pièce, on réalise, avant ou après emboutissage, un composé allié intermétallique, en surface, assurant une protection contre la corrosion, contre la décarburation de l'acier, le composé intermétallique pouvant assurer une fonction de lubrification, on retire par découpage, les excédents de tôle nécessaires à l'opération d'emboutissage. Process for producing a part with very high mechanical characteristics, shaped by stamping, from a strip of rolled steel sheet, in particular hot rolled and coated with a metal or a metal alloy ensuring surface and steel protection, characterized in that : the sheet is cut to obtain a sheet blank, stamping is carried out from the sheet blank to obtain the part, before or after drawing, an alloyed intermetallic compound is produced on the surface, providing protection against corrosion, against decarburization of steel, the intermetallic compound being able to provide a lubrication function, the excess sheet metal necessary for the stamping operation is removed by cutting. Procédé selon la revendication 1 caractérisé en ce que : on découpe la tôle pour l'obtention d'un flan de tôle, on soumet le flan de tôle revêtue à une élévation en température dans le but de former une pièce à chaud, on réalise, de ce fait un composé allié intermétallique, en surface, assurant une protection contre la corrosion, contre la décarburation de l'acier, le composé intermétallique pouvant assurer une fonction de lubrification, on effectue la mise en forme du flan de tôle, par emboutissage, on refroidit la pièce formée pour conférer des caractéristiques mécaniques de dureté élevées de l'acier et une dureté superficielle élevée du revêtement, on retire par découpage, les excédents de tôle nécessaires à l'opération d'emboutissage. Method according to claim 1 characterized in that : the sheet is cut to obtain a sheet blank, the coated sheet metal blank is subjected to a rise in temperature in order to form a hot part, this produces an alloyed intermetallic compound, on the surface, providing protection against corrosion, against decarburization of steel, the intermetallic compound being able to provide a lubrication function, the sheet blank is shaped, by stamping, the formed part is cooled to give mechanical characteristics of high hardness of the steel and a high surface hardness of the coating, the excess sheet metal necessary for the stamping operation is removed by cutting. Procédé selon la revendication 1 caractérisé en ce que le métal ou l'alliage métallique du revêtement est du zinc ou un alliage à base de zinc d'une épaisseur comprise entre 5µm et 30 µm.Process according to Claim 1, characterized in that the metal or the metal alloy of the coating is zinc or a zinc-based alloy with a thickness between 5 µm and 30 µm. Procédé selon la revendication 1 caractérisé en ce que l'alliage intermétallique est un composé à base de zinc-fer ou de zinc-fer-aluminium. Process according to Claim 1, characterized in that the intermetallic alloy is a compound based on zinc-iron or zinc-iron-aluminum. Procédé selon la revendication 1 caractérisé en ce que la tôle revêtue est soumise à une élévation de température supérieure à 700°C avant la mise en forme et ou le traitement thermique.A method according to claim 1 characterized in that the coated sheet is subjected to a temperature rise above 700 ° C before shaping and or heat treatment. Procédé selon la revendication 1 caractérisé en ce que la pièce obtenue notamment par emboutissage est refroidie pour subir une trempe, à une vitesse supérieure à la vitesse critique de trempe.A method according to claim 1 characterized in that the part obtained in particular by stamping is cooled to undergo quenching, at a speed greater than the critical quenching speed. Utilisation d'une bande de tôle d'acier laminée et notamment laminée à chaud et revêtue d'un métal ou d'un alliage métallique assurant une protection de la surface et de l'acier de la tôle dans la mise en forme par emboutissage notamment à chaud de pièces, les pièces ayant de hautes caractéristiques mécaniques en dureté et de hautes caractéristiques de dureté en surface ainsi qu'une très bonne tenue à l'abrasion.Use of a strip of rolled steel sheet, in particular hot rolled and coated with a metal or metal alloy ensuring surface protection and sheet steel in forming by stamping, especially hot parts, the parts having high mechanical characteristics in hardness and high surface hardness characteristics as well as very good abrasion resistance.
    EP01400861A 2000-04-07 2001-04-04 Method for manufacturing a body featuring very high mechanical properties, forming by drawing from a rolled steel sheet, in particular hot rolled and coated sheet Revoked EP1143029B1 (en)

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    DE20122563U DE20122563U1 (en) 2000-04-07 2001-04-04 Workpiece with very high mechanical properties, which has been shaped by deep drawing from a rolled and in particular hot-rolled and coated strip steel sheet
    EP10006299.1A EP2224034B1 (en) 2000-04-07 2001-04-04 Method for manufacturing a body featuring very high mechanical properties, formed by drawing from a rolled steel sheet, in particular hot rolled and coated sheet
    EP06002618.4A EP1672088B2 (en) 2000-04-07 2001-04-04 Method for manufacturing a body featuring very high mechanical properties, forming by cold drawing from a rolled steel sheet, in particular hot rolled and coated sheet

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    FR0004427 2000-04-07
    FR0004427A FR2807447B1 (en) 2000-04-07 2000-04-07 METHOD FOR MAKING A PART WITH VERY HIGH MECHANICAL CHARACTERISTICS, SHAPED BY STAMPING, FROM A STRIP OF LAMINATED AND IN PARTICULAR HOT ROLLED AND COATED STEEL SHEET

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    EP06002618.4A Expired - Lifetime EP1672088B2 (en) 2000-04-07 2001-04-04 Method for manufacturing a body featuring very high mechanical properties, forming by cold drawing from a rolled steel sheet, in particular hot rolled and coated sheet
    EP10006299.1A Revoked EP2224034B1 (en) 2000-04-07 2001-04-04 Method for manufacturing a body featuring very high mechanical properties, formed by drawing from a rolled steel sheet, in particular hot rolled and coated sheet

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    US20010042393A1 (en) 2001-11-22
    CA2343340A1 (en) 2001-10-07
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    EP1672088B1 (en) 2010-08-18
    ES2350399T3 (en) 2011-01-21
    JP3825456B2 (en) 2006-09-27
    DE10006299T1 (en) 2012-01-26
    BR0102747A (en) 2001-12-04
    JP3663145B2 (en) 2005-06-22
    ATE327353T1 (en) 2006-06-15
    ES2350399T5 (en) 2015-11-10
    EP2224034A1 (en) 2010-09-01
    ES2263567T3 (en) 2006-12-16
    EP1672088B2 (en) 2015-01-28
    PT1672088E (en) 2010-11-04
    EP1143029B1 (en) 2006-05-24
    BRPI0117371B1 (en) 2016-06-14
    DE60142859D1 (en) 2010-09-30
    DE01400861T1 (en) 2005-05-04
    FR2807447A1 (en) 2001-10-12
    JP2005047001A (en) 2005-02-24
    DK1143029T3 (en) 2006-09-18
    FR2807447B1 (en) 2002-10-11
    ATE478167T1 (en) 2010-09-15
    EP1672088A1 (en) 2006-06-21
    DE60119826T2 (en) 2006-12-14
    DE20122563U1 (en) 2006-05-11
    DE60119826D1 (en) 2006-06-29
    BRPI0102747B1 (en) 2016-08-30
    CA2343340C (en) 2008-07-08
    EP2224034B1 (en) 2013-07-17
    AR028319A1 (en) 2003-05-07
    PT1143029E (en) 2006-09-29
    ES2428638T3 (en) 2013-11-08

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