EP1565596A1 - Production de couches en chrome dur structurees - Google Patents

Production de couches en chrome dur structurees

Info

Publication number
EP1565596A1
EP1565596A1 EP03773629A EP03773629A EP1565596A1 EP 1565596 A1 EP1565596 A1 EP 1565596A1 EP 03773629 A EP03773629 A EP 03773629A EP 03773629 A EP03773629 A EP 03773629A EP 1565596 A1 EP1565596 A1 EP 1565596A1
Authority
EP
European Patent Office
Prior art keywords
alkali
ammonium
electrolyte
layer
structured
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
EP03773629A
Other languages
German (de)
English (en)
Other versions
EP1565596B1 (fr
Inventor
Rudolf Linde
Stefan Dürdoth
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.)
Federal Mogul Burscheid GmbH
Original Assignee
Federal Mogul Burscheid GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Federal Mogul Burscheid GmbH filed Critical Federal Mogul Burscheid GmbH
Publication of EP1565596A1 publication Critical patent/EP1565596A1/fr
Application granted granted Critical
Publication of EP1565596B1 publication Critical patent/EP1565596B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12389—All metal or with adjacent metals having variation in thickness
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12389—All metal or with adjacent metals having variation in thickness
    • Y10T428/12396—Discontinuous surface component
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12486—Laterally noncoextensive components [e.g., embedded, etc.]
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12778—Alternative base metals from diverse categories
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12826—Group VIB metal-base component
    • Y10T428/12847—Cr-base component
    • 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
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal

Definitions

  • the invention relates to a method for producing a structured hard chrome layer on a workpiece, structured hard chrome layers obtainable thereby and an electrolyte for carrying out the method.
  • Electrochemically or galvanically deposited chrome layers have been the state of the art in functional and decorative areas of application and applications for coating electrically conductive and non-conductive workpieces for many years.
  • the structured layers used according to the prior art all have a pronounced spherical layer structure.
  • the size of the spherical shapes varies between less than 1 ⁇ m and several ⁇ m.
  • the degree of coverage or the density of the spherical layer structure can be varied more or less depending on the method.
  • Structured chrome layers according to DE 33 077 48 A1, DE 42 11 881 A1 and DE 43 34 122 A1 are produced by varying the direct electrical currents, the structure of the structures being influenced by varying the current ramp and current pulse heights.
  • spherical structures are also produced. Here, however, their growth is made possible by adding salts of the elements selenium or tellurium to the chromium plating electrolyte.
  • WO 02/38835 A1 discloses a method for the electrolytic coating of materials, a chromium alloy being deposited from an electrolyte which contains at least chromic acid, sulfuric acid, a metal which forms isopolyanions, a short-chain aliphatic sulfonic acid, its salt and / or its halogenated derivative and Contains fluorides.
  • a structured hard chrome layer is not mentioned in this prior art.
  • the present invention is therefore based on the object of providing a method for producing a structured hard chrome layer which does not have the disadvantages of the prior art.
  • this is achieved by a method for producing a structured hard chrome layer, chrome being deposited from an electrolyte on a workpiece which contains:
  • the method according to the invention is ideally suited to be used for the production of structured hard chrome layers.
  • a structured hard chrome layer is obtained by deliberately influencing the cathode film formed during the electrochemical deposition of metals, the layer being cup-shaped and / or labyrinth-like and / or column-shaped.
  • salts are dissolved in water, they dissociate into cations and anions. These dissociated ions simultaneously surround themselves with a hydration shell, i.e. water molecules (as dipoles) accumulate around the cations or anions. The charge number of the ions is not changed during the hydration. If a hydrated metal ion now begins to migrate under the influence of current, it gets near the cathode in a border area between the electrolyte and the cathode.
  • This so-called cathode film is located directly on the surface of the workpiece to be coated, since the workpiece is switched electrically negative.
  • the metal ions present in the electrolyte are first aligned in this phase boundary by taking up electrons which are offered by the cathode from the electric current.
  • an electrochemical double layer also called "Helmholtz double layer”. It is a name for the electrically charged zone at the electrolyte / electrode interface, which is about a few atomic or molecular layers thick. Its formation is made up of ions and electrons or directed dipole molecules. It is positively charged on one side, negatively charged on the other side and behaves like a plate capacitor with an extremely small plate spacing.
  • the resulting metal atom is now on the workpiece surface, but its condition is not yet the same of an atom in the interior of the metal. Only when a so-called growth site is present do the atoms that are formed fit into the existing metal lattice.
  • the deposition conditions of the electrolytes are usually selected so that the base material is evenly covered with the metal to be deposited.
  • the element chromium is present in aqueous solution, in comparison to most electrochemically separable elements, as a negatively charged complex ion mainly as a hydrogen dichromate in a strongly acidic solution.
  • the chromium in this complex has the oxidation state 6.
  • smaller amounts of chromium (III) compounds are also contained in electrolytes.
  • the formation of the cathode film is controlled in such a way that it becomes permeable to chromium ions, so that a very dense barrier layer first forms, which then breaks down depending on the applied electrical coating current density and the metal structure of different thicknesses or layer thickness can arise.
  • structured chrome layers which are cup-shaped and / or labyrinth-like and / or column-shaped, are obtained.
  • the chrome layer obtained by the process according to the invention has high wear and corrosion resistance, excellent sliding properties and
  • the special structure of the layer ensures better absorption of liquids.
  • the construction of a gas cushion can be made possible and an improved anchoring possibility for substances to be stored there, e.g. Plastics, dyes, metals, ceramics, electronic
  • Components the body's own tissue as an implant coating, can be achieved. Furthermore, this special structure enables targeted optical effects, e.g. high adsorption capacity for light and heat radiation when using
  • electrolyte is understood to mean aqueous solutions whose electrical conductivity is brought about by electrolytically dissociation in ions. Accordingly, the electrolyte has, in addition to components (a) to (d) and any further additives present, the rest of water ,
  • Cr0 3 is preferably used, which has proven to be particularly favorable for the electrodeposition of chromium.
  • An aliphatic sulfonic acid which is preferably used as component (c) is methanesulfonic acid. This has proven to be particularly favorable for the formation of the structured hard chrome layers with the above properties.
  • component (d) Li * . Na + and K + can be used.
  • alkaline earth metal ions are Mg 2 * and Ca 2 ⁇ .
  • component (d) (NH 4 ) 6 M ⁇ 7 ⁇ 2 -4 H 0, which has been found to be particularly favorable for the formation of the structured hard chrome layer with the above properties Has.
  • the electrolyte described in more detail above is essentially free of fluorides.
  • fluorides are understood to be both simple and complex fluorides. If fluoride is present in the electrolyte, the formation of the structured hard chrome layer is disturbed. The expression “essentially no fluorides” therefore means that so much fluoride is tolerable in the electrolyte that the formation of the structured hard chrome layer is not influenced. The amount of fluorides that are tolerable can easily be determined by a person skilled in the art. It has proven to be advantageous proven if there is no more than 0.1 g / l in the electrolyte.
  • the electrolyte can also contain conventional catalysts that support chromium deposition, such as S0 4 2 " and / or CI " . These can be present in the electrolyte in conventional amounts.
  • structured hard chrome layers are formed on workpieces.
  • workpiece is understood to mean objects of any kind that are to be provided with a structured chrome layer. These can be metallic or non-metallic objects. Should a non-metallic object be used structured hard chrome layer are formed, this is first made electrically conductive by applying a thin metal film.
  • the structured hard chrome layer on the workpiece is switched cathodically and immersed in the electrolyte.
  • a direct current for example a pulsating direct current with a frequency of up to 1000 Hz, is applied to the workpiece.
  • the temperature for the deposition of chromium can be 45 ° C to 95 ° C, in particular about 55 ° C.
  • the duration of the deposition is chosen depending on the desired thickness of the structured hard chrome layer, the layer becoming thicker the longer the deposition takes place.
  • a current density of 20 A / dm 2 to 200 A / dm 2 is used. In this way, particularly favorable structures of the hard chrome layer are obtained. The higher the current density selected, the denser the protruding areas of the structured hard chrome layer.
  • the cathodic current yield in the production of the structured hard chrome layer according to the method according to the invention is 12% or less. If the current yield is higher, the desired structuring of the hard chrome layer is not obtained.
  • the structured hard chrome layer obtainable by the method according to the invention can first be applied to a workpiece and then a layer selected from a conventional chrome layer, black chrome layer, copper, nickel or tin layer.
  • a conventional chrome, copper and / or nickel layer can first be applied to the workpiece and the hard chrome layer described in more detail above can be deposited thereon.
  • non-chromium-containing coatings such as copper, nickel, tin, zinc, ceramic, plastic, solid lubricants, dyes, can be applied directly to the hard chrome layer obtainable by the process according to the invention.
  • the present invention also relates to a structured hard chrome layer, as can be obtained by the inventive method described in more detail above.
  • the structured hard chrome layer is cup-shaped and / or labyrinth-like and / or column-shaped.
  • the structured hard chrome layer according to the invention has the advantages described in connection with the method according to the invention.
  • the structured hard chrome layer according to the invention can be used to coat a large number of workpieces, for example piston rings, cylinders, pistons, bolts, camshafts, seals, composite materials, valves, bearings for protection against wear and to reduce friction, pressure cylinders for better wetting with paints, embossing rollers for better deep-drawing processes for the automotive industry, in solar technology, for decorative applications, in medical technology, microtechnology and microelectronics.
  • workpieces for example piston rings, cylinders, pistons, bolts, camshafts, seals, composite materials, valves, bearings for protection against wear and to reduce friction
  • pressure cylinders for better wetting with paints
  • embossing rollers for better deep-drawing processes for the automotive industry, in solar technology, for decorative applications, in medical technology, microtechnology and microelectronics.
  • the present invention also relates to an electrolyte containing
  • This electrolyte can be used in particular for producing the structured hard chrome layers on workpieces described in more detail above.
  • Figures 1 to 8 show photographs according to the hard chrome layers from Examples 1 to 8.
  • Example 1 shows photographs according to the hard chrome layers from Examples 1 to 8.
  • Example 1 shows photographs according to the hard chrome layers from Examples 1 to 8.
  • the article coated under these conditions has a conventional glossy, evenly formed chrome layer after the treatment, cf. Fig. 1.
  • Ammonium molybdate (NH 4 ) 6 M ⁇ 7 ⁇ 24 • 4 H 2 0 100 g / l and methanesulfonic acid 4 g / l are additionally added to the electrolyte according to example 1.
  • a part of the goods is coated according to the conditions described in Example 1.
  • the article described in this way has a structured chrome layer after the treatment. This chrome layer has a glossy appearance on the protruding surface areas (supporting portion) and brown-colored cathode film or barrier layer is obtained in the recesses of the structure (FIG. 2).
  • Example 3 A part is coated according to the conditions from Example 2. However, instead of a coating current density of 40 A / dm 2 , 20 A / dm 2 is used.
  • the article coated in this way has a structured chrome layer after the treatment.
  • the proportion of the protruding, glossy surface areas (supporting portion) is lower and the proportion of the deep areas is larger in comparison to the structure layer from Example 2 (FIG. 3).
  • a part of the goods is coated according to the conditions of Example 2. However, instead of a coating current density of 40 A / dm 2 , 60 A / dm 2 is used.
  • Example 5 The article coated in this way has a structured chrome layer after the treatment.
  • the proportion of the protruding, glossy surface areas (supporting portion) is greater and the proportion of the deep regions is less in comparison to the structure layer from Example 2 (FIG. 4).
  • Example 5 Example 5:
  • a part of the goods is coated according to the conditions of Example 2.
  • the article coated in this way has a structured chrome layer after the treatment.
  • the product part coated in this way has a considerable increase in the structural height in comparison to example 2 (FIG. 5).
  • This graded layer has metallurgical properties on the surface like conventional chrome and is additionally structured.
  • the advantage of this layer structure is that the profile height of the structural layer can be varied within a wide range, which is limited by the exclusive deposition according to Examples 2-4 and the low layer growth rate.
  • a part of the goods is coated according to the conditions of Example 2.
  • the article coated in this way has a structured chrome layer after the treatment.
  • a black chrome oxide-containing layer is then deposited on this structured chrome layer.
  • the product part coated in this way has a uniform, deep black surface with a very high light calculation index (FIG. 6).
  • a part of the goods is coated according to the conditions of Example 2.
  • the article coated in this way has a structured chrome layer after the treatment.
  • a tin layer is now deposited on this structured chrome layer, of sufficient thickness to fill the recesses in the structured chrome layer with tin.
  • the product part coated in this way has a surface which, with high wear resistance, also has very good sliding properties (FIG. 7).
  • a part of the goods is coated with a conventional chrome layer in accordance with the conditions from Example 1.
  • a structured chrome layer is then applied to the chrome layer from example 1 using the conditions from example 2.
  • the structured chrome layer represents an inlet layer for the conventional chrome layer and, depending on the tribological application, leads to an improvement in the layer system (FIG. 8).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

L'invention concerne un procédé permettant de produire une couche en chrome dur structurée, le chrome étant déposé à partir d'un électrolyte sur une pièce à usiner. Ledit électrolyte contient : (a) des composés Cr(VI), dans une quantité correspondant à entre 50 et 600 g/l d'anhydride d'acide chromique ; (b) entre 0,5 et 10g/l d'acide sulfurique ; (c) entre 1 et 20 g/l d'acide sulfonique aliphatique ayant entre 1 et 6 atomes de carbone, et (d) entre 10 et 200 g/l d'au moins un composé formant un film cathodique dense, ledit composé étant sélectionné parmi : molybdate d'ammonium, d'alcali et molybdate alcalino-terreux, vanadate d'ammonium, d'alcali et vanadate alcalino-terreux et zirconate d'ammonium, d'alcali et zirconate alcalino-terreux. L'invention concerne en outre une couche de chrome dur structurée pouvant être obtenue selon ledit procédé et un électrolyte pour mettre ledit procédé en oeuvre.
EP03773629A 2002-11-29 2003-09-18 Production de couches en chrome dur structurees Expired - Lifetime EP1565596B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10255853 2002-11-29
DE2002155853 DE10255853A1 (de) 2002-11-29 2002-11-29 Herstellung strukturierter Hartchromschichten
PCT/EP2003/010425 WO2004050960A1 (fr) 2002-11-29 2003-09-18 Production de couches en chrome dur structurees

Publications (2)

Publication Number Publication Date
EP1565596A1 true EP1565596A1 (fr) 2005-08-24
EP1565596B1 EP1565596B1 (fr) 2006-08-09

Family

ID=32318822

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03773629A Expired - Lifetime EP1565596B1 (fr) 2002-11-29 2003-09-18 Production de couches en chrome dur structurees

Country Status (8)

Country Link
US (2) US7699970B2 (fr)
EP (1) EP1565596B1 (fr)
JP (1) JP4373923B2 (fr)
AU (1) AU2003282018A1 (fr)
BR (1) BRPI0315192B1 (fr)
DE (2) DE10255853A1 (fr)
PT (1) PT1565596E (fr)
WO (1) WO2004050960A1 (fr)

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DE102005022692A1 (de) * 2005-05-18 2006-11-23 Robert Bosch Gmbh Verfahren zur Herstellung beschichteter Oberflächen und Verwendung derselben
DE102006042076A1 (de) * 2006-09-05 2008-03-20 Goldschmidt Tib Gmbh Ein neues Additiv für Chromelektrolyte
DE102008017270B3 (de) * 2008-04-04 2009-06-04 Federal-Mogul Burscheid Gmbh Strukturierte Chrom-Feststoffpartikel-Schicht und Verfahren zu deren Herstellung sowie beschichtetes Maschinenelement
AT507785B1 (de) 2009-08-04 2010-08-15 Univ Wien Tech Verfahren zur herstellung strukturierter chromschichten
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DE102011084051B4 (de) 2011-10-05 2020-03-12 Federal-Mogul Burscheid Gmbh Beschichteter Kolbenring mit radial zunehmender Schichtdicke und Verfahren zu dessen Herstellung
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JP2006508243A (ja) 2006-03-09
BRPI0315192B1 (pt) 2015-10-13
DE50304610D1 (de) 2006-09-21
WO2004050960A1 (fr) 2004-06-17
US20060054509A1 (en) 2006-03-16
PT1565596E (pt) 2006-12-29
DE10255853A1 (de) 2004-06-17
BR0315192A (pt) 2005-08-23
US7699970B2 (en) 2010-04-20
AU2003282018A1 (en) 2004-06-23
JP4373923B2 (ja) 2009-11-25
US20100112376A1 (en) 2010-05-06
US8277953B2 (en) 2012-10-02
EP1565596B1 (fr) 2006-08-09

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