EP1213372B1 - Procédé et disposition pour la déposition galvanique de nickel, cobalt, d'alliages de nickel ou de cobalt grâce à des impulsions périodiques de courant et utilisation de ce procédé - Google Patents

Procédé et disposition pour la déposition galvanique de nickel, cobalt, d'alliages de nickel ou de cobalt grâce à des impulsions périodiques de courant et utilisation de ce procédé Download PDF

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Publication number
EP1213372B1
EP1213372B1 EP01128897A EP01128897A EP1213372B1 EP 1213372 B1 EP1213372 B1 EP 1213372B1 EP 01128897 A EP01128897 A EP 01128897A EP 01128897 A EP01128897 A EP 01128897A EP 1213372 B1 EP1213372 B1 EP 1213372B1
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Prior art keywords
nickel
cobalt
deposition
anode
electrolyte
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German (de)
English (en)
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EP1213372A2 (fr
EP1213372A3 (fr
Inventor
Rüdiger Ewald
Peter Filke
Michael Heckmann
Wolfgang Keinath
Günter Langel
Anton Schmidt
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Airbus DS GmbH
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Astrium GmbH
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/008—Current shielding devices
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10—Electrodes, e.g. composition, counter electrode
    • C25D17/12—Shape or form
    • 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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • 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
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/18—Electroplating using modulated, pulsed or reversing current

Definitions

  • the present invention relates to a process for the electrodeposition of nickel, cobalt, nickel alloys or cobalt alloys in a galvanic bath using a nickel compounds or cobalt compounds such as electrolytes containing sulfates or sulfamates or chlorides.
  • Such electrolytes for electrodeposition are for example made DE 25 58 423 . DE 22 18 967 . US 2,470,775 such as EP 0 835 335 known.
  • At least one anode and at least one cathode of the bath is subjected to periodic current pulses.
  • Such methods with the aid of current pulses are known from the prior art, for example, from the already mentioned publications US 2,470,775 such as EP 0 835 335 known. From the US-A-3,915,835
  • the object of the present invention is therefore to provide a method for the electrodeposition of nickel, cobalt, nickel alloys or cobalt alloys in a galvanic bath, in which at least one anode and at least one cathode of the bath is subjected to periodic current pulses and with the nickel or cobalt layers or layers of a nickel or cobalt alloy can be produced, which can be permanently connected to other components, in particular can be welded to other components.
  • an electrolyte which contains corresponding nickel compounds or cobalt compounds, in particular sulfates or sulfamates or chlorides.
  • a cathode of the bath ie a so-called pulse plating process is used.
  • a cathode normally acts a deposition body on which a layer of the corresponding material to be deposited.
  • the ratio I A / I C is between 1.2 and 1.45, in particular between 1.3 and 1.4, and the charge ratio Q A / Q C - (T A * I A ) / (T C ⁇ I C ) is between 35% and 40%.
  • particularly advantageous properties of the deposited layer can be determined, in particular with regard to the strength and the extensibility.
  • At least one contoured anode is used for the deposition, the contour of which is aligned with the contour of the deposition body on which the nickel, the cobalt, the nickel government or the cobalt alloy is deposited is.
  • a contoured anode is used for at least one of the anodes located closest to the deposition body.
  • the effect of contouring the anode is more pronounced than for more remote anodes, i. that anodes without contouring can be used for these more remote anodes, which may be more cost-effective and can be used independently of the specific shape of the deposition body.
  • a contoured container permeable to the ions of the nickel or cobalt to be deposited or the nickel alloy or cobalt alloy and filled with bodies of nickel, cobalt or a nickel alloy or cobalt alloy may be used.
  • Special containers for such bodies are basically made DE 25 58 423 in the form of titanium or plastic baskets which are filled there with nickel pellets, but there is no contouring of the container is provided.
  • a solid electrode body which has at least one coating of the nickel, cobalt or the nickel alloy or cobalt alloy to be deposited or, in principle, consists of solid nickel, cobalt or a solid nickel alloy or cobalt alloy can also be used as the contoured anode.
  • a targeted influencing of the deposition is necessary, which should be different for different areas of the deposition body.
  • This influencing can take place additionally or else alternatively to the aforementioned measure of the contoured anodes.
  • the deposition body is at least partially shielded by current shutters during a part of the entire deposition period. In the shielded areas, a reduced deposition is then achieved as compared to the unshielded areas during the time these areas are shielded.
  • layer properties in particular the layer thickness, but possibly also the mechanical layer properties, can be realized on the deposition body.
  • the current shutters can be arranged in those regions of the deposition body in which a preferred deposition takes place.
  • an excessive layer growth in these areas can be prevented in comparison to other areas and thus a more homogeneous layer growth can be realized over the entire deposition body.
  • a cleaning of the electrolyte with the aid of activated carbon and / or hydrogen peroxide take place.
  • 0.5 g / l to 5 g / l, in particular 1 g / l to 3 g / l of activated carbon can be used to purify the electrolyte and 0.5 ml / l to 3 ml / l, in particular 1 ml / l before the deposition to 2ml / l of 30% hydrogen peroxide.
  • Purification of the electrolyte take place alternatively or additionally during the deposition.
  • filtering of the electrolyte for example by means of activated carbon filters, is provided for this purpose during the deposition on the one hand, and on the other hand foreign elements are removed from the electrolyte by a selective bath.
  • a selective bath corresponds to a galvanic bath, in which a targeted separation of foreign elements and thus their removal from the electrolyte takes place by targeted control of the currents.
  • the thus purified electrolyte then ideally contains only the desired elements, in the case of a nickel electrolyte then ideally only nickel or nickel alloys in the compounds mentioned above, in the case of a cobalt electrolyte ideally only cobalt or cobalt alloys in the compounds mentioned above ,
  • the purified electrolyte is then returned to the galvanic bath.
  • nozzles can now in particular be designed and arranged in the bath such that a circulation of the bath is favored by the nozzles and / or a flow of the electrolyte directed onto the deposition body is achieved.
  • the nozzles not only fulfill the purpose of circulation and return of the electrolyte in the bath, but by this optimized type of recycling, the deposition process in the bath favors, as always optimal mixing or targeted supply of a pure electrolyte as possible to the deposition body is guaranteed.
  • the inventive method is basically suitable for the production of different components that are later inextricably linked to other components, for example, to be welded.
  • the method is particularly suitable for the production of components that are exposed to high loads. This applies, for example, to components for rocket engines, in which case in particular the application of the method for the production of injection heads and / or combustion chambers and / or thrusters for rocket engines is called.
  • the method can also be used for other components that are subject to high loads in later operation, and therefore must have sufficient strength, but nevertheless should have sufficient extensibility, such as supporting mechanical structures, components for kilns or similar arrangements with high thermal stress, etc.
  • the achievable strength as well as the extensibility of the deposited layer over a relatively wide range is adjustable, as will be explained in more detail below.
  • This special galvanic bath can be used to implement a specific development of the aforementioned method.
  • the aforementioned method can in principle but also in otherwise trained galvanic Baths are realized, which are suitably adapted to the basic inventive method or one of its developments.
  • the at least one contoured anode is formed as a contoured container which can be filled with bodies of nickel or cobalt or a nickel alloy or a cobalt alloy.
  • a plurality of anodes are arranged in the bath, wherein only the anodes closest to the deposition body are formed as contoured anodes.
  • the other anodes also have a certain contour, but in this case, only the contour of those anodes which are closest to the deposition body should be adapted to the contour of the deposition body.
  • the contouring can only be done in one spatial direction e.g. in the longitudinal direction of the anode, or it can also take place in more than one spatial direction, e.g. additionally perpendicular to the longitudinal direction.
  • the cleaning device may include a filter device, in particular an activated carbon filter, and a Selektivbad.
  • a filter device in particular an activated carbon filter
  • Selektivbad a Selektivbad
  • a galvanic bath with an electrolyte is provided in the context of the following example, which contains nickel compounds.
  • a galvanic bath with cobalt compounds is conceivable.
  • electrolytes as nickel compounds or cobalt compounds, for example, nickel sulfate and nickel chloride or nickel sulfamate and nickel chloride can be provided, and in the case of cobalt compounds, the corresponding sulfates, sulfamates or chlorides.
  • the composition of the electrolyte reference is made to the cited prior art.
  • additional additives in the electrolyte such as that in US Pat EP 0 835 335 or DE 22 18 967 quoted sulfonated naphthalene or the in US 2,470,775 Column 3, paragraph 2.
  • pulse plating is now used for the deposition, that is, the charging of the anodes and cathodes of the bath with periodic current pulses, which is known in principle from the cited prior art.
  • periodic current pulses which is known in principle from the cited prior art.
  • Fig. 1 determines the dependence of the yield strength (0,2-proof stress) R p 0,2 .
  • Fig. 2 shows schematically the construction of the bath for the realization of the invention, which is filled with an electrolyte as described above.
  • a deposition body 2 such as a combustion chamber of a rocket engine in a bath 1.
  • a coating for example, nickel galvanically generated.
  • at least one anode 3 is embedded in the bath 1, wherein the anode 3 is contoured such that it is adapted to the contour of the deposition body 2.
  • the contouring can be given only in one spatial direction, for example in the longitudinal direction of the anode 3, or it can also be provided in more than one spatial direction, for example additionally perpendicular to the longitudinal direction.
  • FIG. 3 shows a possible arrangement of several anodes 3a, 3b in a bath 1, wherein those anodes 3a, which are closest to the deposition body, are formed as contoured anodes, since there makes the positive influence of the contouring most noticeable.
  • the more remote anodes 3b can be designed as universally usable, in the simplest case flat anodes, for which any standardized anode form can be used. Consequently, only the anode 3 a closest to the deposition body 2 may need to be adapted to the specific shape of different deposition bodies 2.
  • This anode concept represents an optimization of the effect of the anodes 3a, 3b while maintaining a possible universal arrangement.
  • the contoured anode 3 in Fig. 2 is formed by a contoured container 8, which is formed for example as a titanium basket and therefore permeable is for the necessary for the deposition of nickel ions.
  • the container 8 may also be surrounded by additional, likewise permeable to the nickel ions sheaths such as from a bag.
  • the nickel is introduced here in the form of small nickel bodies 9 in the container 8 and can be easily replenished in a simple manner with a gradual consumption of nickel during the deposition process.
  • a device 4 activates the anode 3 and the deposition body 2 acting as a cathode in the bath 1 with periodic current pulses for carrying out the described pulse plating process.
  • the current apertures 5 which shield certain areas of the deposition body 2 at least during part of the deposition process.
  • the edges of the deposition body 2 are shielded, since in these areas without shielding an increased deposition of the nickel would take place and so an inhomogeneous deposition would take place over the entire deposition body 2.
  • the current apertures 5 should be provided as rings, which are arranged concentrically around the edge regions of the deposition body 2. By means of the current diaphragms 5, these regions can be shielded, at least over a certain time, so that a more homogeneous deposition over the entire deposition body 2 can be achieved over the entire deposition period.
  • the deposition body 2 can be shielded analogously, the corresponding areas in which an increased deposition takes place, such as surveys. Thus, an otherwise lower deposition in other areas such as wells can be compensated.
  • the current sheds 5 can for example be arranged displaceably or even completely removable in the bath 1, for which purpose suitable devices are to be provided.
  • a cleaning device 6 is used to clean the electrolyte of interfering foreign elements and suspended particles during the deposition process and takes place with the aid of activated carbon filters 10 and a selective bath 11, in Fig. 2 only shown schematically.
  • the discharge and return of the electrolyte in the bath is carried out by appropriate supply and discharge lines.
  • the bathroom also has a in Fig. 2 schematically shown circulating device 13 for circulating the electrolyte, which consists of a circulation pump 12 and suitably designed and suitably arranged nozzles 7 for recycling the electrolyte.
  • a circulation pump 12 for circulating the electrolyte
  • nozzles 7 for recycling the electrolyte.
  • the appropriate arrangement and orientation of the nozzles 7 should be chosen so that these specifications are met.
  • the cleaning device 6 and the circulation device 13 could also be combined in a single device, for example by recycling the electrolyte purified in the cleaning device 6 into the bath 1 with the aid of nozzles 7.

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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 Methods And Accessories (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Claims (19)

  1. Procédé de dépôt de nickel, cobalt, alliages de nickel ou alliages de cobalt par galvanisation dans un bain de galvanisation (1) en recourant à un électrolyte qui contient des composés du nickel ou des composés du cobalt,
    dans lequel des impulsions de courant sont appliquées périodiquement sur au moins une anode (3, 3a, 3b) et au moins une cathode du bain (1) pour déposer du nickel, du cobalt, des alliages de nickel ou des alliages de cobalt sur un corps de dépôt (2) et
    dans lequel le corps de dépôt (2) joue le rôle d'une anode ou d'une cathode,
    caractérisé en ce que
    le rapport IA/IC entre la densité de courant IA à l'anode et la densité de courant IC à la cathode est sélectionné à une valeur supérieure à 1 et inférieure à 1,5,
    en ce que le rapport QA/QC = (TA-IA)/(TC/IC) entre la charge QA transportée pendant une impulsion d'anode de durée TA et la charge QC transportée pendant une impulsion de cathode de durée TC est compris entre 30 % et 45 % et
    en ce que la densité IA de courant à l'anode et la densité IC du courant à la cathode sont définies comme étant les densités de courant pendant la phase anodique ou la phase cathodique des impulsions de courant sur le corps de dépôt (2).
  2. Procédé selon la revendication 1, caractérisé en ce que le rapport IA/IC est compris entre 1,2 et 1,45, en particulier entre 1,3 et 1,4 et en ce que le rapport QA/QC = (TA-IA)/(TC/IC) entre les charges est compris entre 35 % et 40 %.
  3. Procédé selon l'une des revendications 1 ou 2, caractérisé en ce qu'il utilise pour le dépôt au moins une anode profilée (3, 3a, 3b) dont le profil est adapté au profil du corps de dépôt (2) sur lequel le nickel ou le cobalt, l'alliage de nickel ou l'alliage de cobalt doivent être déposés.
  4. Procédé selon la revendication 3, caractérisé en ce que plusieurs anodes (3, 3a, 3b) sont prévues dans le bain (1) et en ce qu'il utilise une anode profilée (3a) pour l'anode (3a) disposée le plus près du corps de dépôt (2).
  5. Procédé selon l'une des revendications 3 ou 4, caractérisé en ce que pour former l'anode profilée (3a), il utilise un récipient profilé (8) qui est perméable au nickel, au cobalt, à l'alliage de nickel ou à l'alliage de cobalt qui doivent être déposés et qui est rempli par des corps (9) en nickel, en cobalt, en alliage de nickel ou en alliage de cobalt.
  6. Procédé selon l'une des revendications 3 ou 4, caractérisé en ce que comme anode profilée (3, 3a, 3b), il utilise un corps massif d'électrode qui présente au moins un revêtement en nickel ou cobalt à déposer ou en alliage de nickel ou alliage de cobalt à déposer.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce qu'au moins pendant une partie de la durée totale de dépôt, le corps de dépôt (2) est partiellement protégé par des écrans (5) pare-courant.
  8. Procédé selon la revendication 7, caractérisé en ce que les écrans pare-courant (5) sont disposés dans les parties du corps de dépôt (2) dans lesquelles a lieu un dépôt préférentiel.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que l'électrolyte est purifié avant le début du dépôt et/ou pendant le dépôt.
  10. Procédé selon la revendication 9, caractérisé en ce que pour purifier l'électrolyte avant le début du dépôt, il utilise de 0,5 g/l à 5 g/l et en particulier de 1 g/l à 3 g/l de charbon actif et de 0,5 ml/l à 3 ml/l et en particulier de 1 ml/l à 2 ml/l de peroxyde d'hydrogène à 30 %.
  11. Procédé selon l'une des revendications 9 ou 10, caractérisé en ce que pour la purification de l'électrolyte pendant le dépôt, il réalise une filtration de l'électrolyte, en particulier à l'aide d'au moins un filtre (10) à charbon actif, et une élimination des éléments étrangers de l'électrolyte à l'aide d'au moins un bain sélectif (11).
  12. Procédé selon l'une des revendications 1 à 11, caractérisé en ce qu'au moins pendant une partie de la durée du dépôt, l'électrolyte est recyclé à l'aide d'au moins une installation de recyclage (13) et en ce que l'électrolyte est renvoyé dans le bain (1) au moyen d'ajutages (7).
  13. Procédé selon la revendication 12, caractérisé en ce que les ajutages (7) sont configurés et disposés dans le bain (1) de manière à obtenir une recirculation du bain (1) et/ou un écoulement d'électrolyte orienté sur le corps de dépôt (2).
  14. Utilisation d'un procédé selon l'une des revendications 1 à 13 pour la fabrication de composants de propulseurs de fusée.
  15. Utilisation d'un procédé selon l'une des revendications 1 à 13 pour la fabrication de têtes d'injection, de chambres de combustion et/ou de tuyères de poussée de propulseurs de fusée.
  16. Bain de galvanisation (1) destiné au dépôt de nickel, d'alliages de nickel, de cobalt ou d'alliages de cobalt par galvanisation et présentant :
    - un électrolyte qui contient des composés du nickel ou des composés du cobalt destinés à être déposés sur un corps de dépôt (2) et présentant au moins une anode profilée (3, 3a, 3b) dont le profil est adapté au profil du corps de dépôt (2),
    - un système (4) de commande de l'application périodique d'impulsions de courant sur l'anode (3, 3a, 3b) et une cathode (2) du bain (1) dans un rapport IA/IC supérieur à 1 et inférieur à 1,5 et un rapport QA/QC = (TA-IA)/(TC/IC) entre les charges compris entre 30 % et 45 %,
    - des écrans (5) pare-courant qui protègent au moins en partie le corps de dépôt (2),
    - un système d'épuration (6) qui épure l'électrolyte et
    - un système de recirculation (13) qui recycle l'électrolyte et qui présente au moins une pompe de recirculation (12) et des tuyères (7) de renvoi de l'électrolyte dans le bain,
    la densité IA de courant à l'anode et la densité IC du courant à la cathode étant définies comme étant les densités de courant pendant la phase anodique ou la phase cathodique des impulsions de courant sur le corps de dépôt (2).
  17. Bain de galvanisation selon la revendication 16, caractérisé en ce que la ou les anodes profilées (3, 3a, 3b) sont configurées comme récipients profilés (8) qui peuvent être remplis par des corps (9) en nickel, en cobalt, en alliage de nickel ou en alliage de cobalt.
  18. Bain de galvanisation selon l'une des revendications 16 ou 17, caractérisé en ce que plusieurs anodes (3, 3a, 3b) sont disposées dans le bain (1) et en ce que seules les anodes (3a) situées le plus près du corps de dépôt (2) sont configurées comme anodes profilées.
  19. Bain de galvanisation selon l'une des revendications 16 à 18, caractérisé en ce que le système d'épuration (6) contient un système de filtration (10) et un bain sélectif (11).
EP01128897A 2000-12-07 2001-12-05 Procédé et disposition pour la déposition galvanique de nickel, cobalt, d'alliages de nickel ou de cobalt grâce à des impulsions périodiques de courant et utilisation de ce procédé Expired - Lifetime EP1213372B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10061186 2000-12-07
DE10061186A DE10061186C1 (de) 2000-12-07 2000-12-07 Verfahren und Anordnung zur galvanischen Abscheidung von Nickel, Kobalt, Nickellegierungen oder Kobaltlegierungen mit periodischen Strompulsen und Verwendung des Verfahrens

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EP1213372A2 EP1213372A2 (fr) 2002-06-12
EP1213372A3 EP1213372A3 (fr) 2004-02-04
EP1213372B1 true EP1213372B1 (fr) 2011-02-09

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US (1) US6790332B2 (fr)
EP (1) EP1213372B1 (fr)
JP (1) JP4285932B2 (fr)
AT (1) ATE498026T1 (fr)
DE (2) DE10061186C1 (fr)
RU (1) RU2281990C2 (fr)

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CN103526246A (zh) * 2013-09-26 2014-01-22 沈阳化工大学 一种发动机转子表面复合Al-Ni镀层的方法
CN103556192B (zh) * 2013-10-09 2016-03-30 北京航空航天大学 一种采用双向脉冲电源制备具有高力学性能电铸镍层的方法
GB2528873A (en) * 2014-07-31 2016-02-10 Mohammad Sakhawat Hussain Direct high speed nickel plating on difficult to plate metals
RU2617470C1 (ru) * 2015-12-28 2017-04-25 Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университе имени Д. И. Менделеева (РХТУ им. Д. И. Менделеева) Способ электроосаждения покрытий никель-фосфор
CN105862093B (zh) * 2016-05-26 2018-03-06 安庆师范大学 一种离子液体中电镀Ni‑Cr‑PTFE复合镀层的方法

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RU2281990C2 (ru) 2006-08-20
DE10061186C1 (de) 2002-01-17
JP2002226991A (ja) 2002-08-14
DE50115791D1 (de) 2011-03-24
US6790332B2 (en) 2004-09-14
ATE498026T1 (de) 2011-02-15
US20020084190A1 (en) 2002-07-04
JP4285932B2 (ja) 2009-06-24
EP1213372A2 (fr) 2002-06-12
EP1213372A3 (fr) 2004-02-04

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