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EP1060291B1 - Procede pour produire un revetement de protection contre la corrosion et systeme en couches pour substrats en metal leger - Google Patents

Procede pour produire un revetement de protection contre la corrosion et systeme en couches pour substrats en metal leger Download PDF

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Publication number
EP1060291B1
EP1060291B1 EP99911717A EP99911717A EP1060291B1 EP 1060291 B1 EP1060291 B1 EP 1060291B1 EP 99911717 A EP99911717 A EP 99911717A EP 99911717 A EP99911717 A EP 99911717A EP 1060291 B1 EP1060291 B1 EP 1060291B1
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EP
European Patent Office
Prior art keywords
layer
accordance
conductive
layers
substrate
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.)
Expired - Lifetime
Application number
EP99911717A
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German (de)
English (en)
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EP1060291A2 (fr
Inventor
Andreas Dietz
Volker Von Der Heide
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Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Classifications

    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • B05D5/067—Metallic effect
    • B05D5/068—Metallic effect achieved by multilayers
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1886—Multistep pretreatment
    • C23C18/1889—Multistep pretreatment with use of metal first
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing

Definitions

  • the invention relates to a method for producing a corrosion-protecting Coating for a substrate made of a light metal or Light metal alloy.
  • Light metals especially aluminum, find their low specific gravity in more and more technologies. Disadvantageous is that they are very electrochemically base in character are susceptible to corrosion. They are therefore covered with anti-corrosion layers of all kinds. A known method of this type exists in metal layers without current or galvanically on the light metal to separate. This is particularly interesting if there are additional high ones decorative demands are placed on the surface.
  • DE 196 21 881 A1 therefore proposes using a method for Chromium-plating car rims from an aluminum alloy first one Apply a primer coat of powder or wet paint, then the rim dry, apply a layer of plastic wet varnish, dry again and finally to carry out galvanic chrome plating. This different process steps are quite complex and require multiple relocation of the intermediate products to other devices. in addition comes the time it takes to dry
  • a method known from DE 195 39 645 A1 works in a similar manner. Even there a light alloy rim for motor vehicle wheels is coated, namely This rim is initially given a full paint job. Beyond that Intermediate coating as powder coating or as bright nickel plating trained to level the surface structure. This will make it smooth Basis for an electrodeposable, finally deposited decorative gloss metallization created.
  • This layer system offers sufficient corrosion protection for as long as the aluminum substrate as there is no mechanical in the layer There is damage that affects the metal substrate.
  • chromium is a chemically very base metal
  • passivation the formation of a thin oxide layer on the surface
  • Oxygen is then reduced on this surface, which is very large compared to the aluminum exposed by the damage.
  • the oxidation process is the conversion of metallic aluminum to Al 3+ . Due to the very large cathode surface of the chromium oxide, the corrosion of the aluminum at this damaged point is dramatic. One speaks here of a catastrophic failure of the corrosion protection layer.
  • the object of the present invention is to provide an alternative method for Manufacture of a corrosion protective coating for a substrate to propose a light metal and a corresponding layer system that is less sensitive to such damage.
  • This object is achieved by a method for producing a Corrosion protection coating for a substrate made of a light metal or a light metal alloy, in which a first on the substrate electrically non-conductive first layer is applied, the non-conductive first layer generated by anodic oxidation of the substrate later, a densification of the non-conductive by anodic Oxidation occurs first layer, then on the not conductive first layer, a metallized layer is applied without current and a third layer is later applied to the metallic second layer.
  • a layer system comprising a Substrate made of light metal or a light metal alloy, but not one conductive first layer, which consists of an oxide of the substrate material, thereon a currentless applied second layer of one or more metals, a third layer.
  • the third layer is particularly preferably one decorative third layer.
  • the invention makes use of the knowledge that the A prerequisite for the catastrophic failure of the known layer systems the electrical conductivity between anode and cathode at Oxidation process after the damage is.
  • the electrical conductivity is now at precisely this point reliably prevented.
  • the electrode flow is not electrically conductive layer between the substrate on the one hand and the outer layers otherwise provided.
  • These outer layers can be both previous corrosion protection properties continue to be good Have functioned with undamaged shift systems, and they on the other hand, the decorative effects like a glossy chrome layer own and / or be wear-resistant and / or low-friction.
  • the electrically non-conductive layer can by physical methods. for example PVD (physical vapor deposition) or plasma CVD (chemical vapor deposition), through simple polymer layers, i.e. lacquers, or through electrochemical processes are generated.
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • non-conductive layer is replaced by anodic Oxidation of the substrate is generated.
  • the substrate is, as is preferred, aluminum
  • the is not used for the production conductive layer uses an anodizing process. It just becomes that Metal substrate switched as an anode and by applying a voltage Oxidized surface. This oxide layer is chemically relatively inert and forms an ideal electrical one, especially after appropriate post-treatments Barrier.
  • This non-conductive first layer here the oxide layer
  • a metal layer is preferably made using an electroless method Nickel, copper or another metal that can be deposited without current, upset.
  • Copper can then be applied to this metal layer using galvanic processes Flattening of the still rough surface for mechanical Equalization of tension or also applied as a shine, also nickel similar purposes and in particular for additional corrosion protection conceivable.
  • the decorative layer can then also be applied to this layer in the prior art lying layer, in particular chrome, are applied.
  • a very successful and advantageous method is preferably used here. This is because it is the layer created by anodic oxidation, in the case of aluminum it is the anodized layer. post-compressed. This is because the process of oxidation creates pores that should be reduced in size to prevent the non-conductive layer from being destroyed and possibly creating conductive bridges. This post-compression can be done using various methods, one of which is the so-called hot water compression. By immersing it in boiling water, the resulting anhydrous Al 2 O 3 is converted into a boehmite type Al 2 O 3 x H 2 O. This leads to an increase in the volume of the material around the pores, so that the pores shrink themselves.
  • a Activation in the sense of a metallization of non-conductive surfaces is in in this case by applying conductive nuclei possible. Preference is given to a noble metal seed as the crystallization seed used, especially conductive palladium seeds.
  • These palladium nuclei or other crystallization nuclei are during the Compaction applied to the surface and penetrate into the pores during their downsizing.
  • FIG. 1 shows a layer system in a very schematic form.
  • a substrate 5 consists of a light metal or a light metal alloy, in particular aluminum.
  • it can be a light alloy rim for a motor vehicle.
  • An electrically non-conductive first layer 10 is closed on the substrate 5 recognize, in particular an oxide from the material of the substrate 5 can, for example alumina.
  • the aluminum oxide can by means of a Anodizing process have been generated.
  • Another metallic intermediate layer follows the second layer 20 25, which are particularly rough in order to level the usually relatively rough Surface of electrolessly deposited layers 20 is used.
  • the intermediate layer 25 is in particular electrodeposited. This leads to to slight material differences between the second layer 20 and the Intermediate layer 25, even if both e.g. should consist of nickel, because chemically deposited electroless nickel Phosphorus or Contains boron components but does not contain galvanically deposited nickel. For the functionality of the layer system does not matter.
  • a layer 30 follows the intermediate layer 25, For example, a glossy chrome layer that the decorative the outside and / or low-friction and / or wear-resistant properties of the finished Product.
  • a glossy chrome layer that the decorative the outside and / or low-friction and / or wear-resistant properties of the finished Product.
  • a bright chrome layer is applied.
  • the layer be special wear-resistant, hard chrome would be considered.
  • low-friction exterior decorative layers of nickel teflon or lead for low-friction exterior decorative layers of nickel teflon or lead.
  • FIG. 2 the boundary area between layers 10 and 20 is greatly enlarged during the manufacturing process, but is again shown schematically.
  • the non-conductive and in particular by anodic oxidation of the substrate 5 generated first layer 10 has a surface 12.
  • This surface 12 is however not completely flat, but has a large number of pores 13; this is, in particular, the production-related result of carrying out a Anodizing process.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)
  • Chemically Coating (AREA)
  • Electroplating Methods And Accessories (AREA)

Claims (18)

  1. Procédé de fabrication d'un revêtement anticorrosion pour un substrat en métal léger ou en alliage léger, dans lequel
    on dépose tout d'abord sur le substrat (5) une première couche électriquement non conductrice (10), la première couche non conductrice (10) étant réalisée par oxydation anodique du substrat (5),
    on réalise après une densification ultérieure de la première couche non conductrice (10) obtenue par oxydation anodique,
    ensuite on dépose par voie autocatalytique sur la première couche non conductrice (10) une couche métallisée (20),
    et après, sur la deuxième couche métallique (20), on dépose une troisième couche (30).
  2. Procédé selon la revendication 1, caractérisé en ce que l'on utilise comme substrat (5) l'aluminium ou le magnésium ou un alliage employant au moins l'un de ces deux métaux légers.
  3. Procédé selon la revendication 2, caractérisé en ce que l'on utilise comme substrat (5) l'aluminium et, pour produire la première couche non conductrice (10), un procédé d'anodisation.
  4. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'on effectue aussi, en même temps que la densification, une activation par dépôt de germes de cristallisation conducteurs (18) sur la surface (12) ou dans les pores (13) résultant de l'oxydation anodique dans la surface (12) de la première couche (10).
  5. Procédé selon la revendication 4, caractérisé en ce que l'on utilise comme germes de cristallisation conducteurs (18) des germes de métaux précieux, en particulier des germes de palladium.
  6. Procédé selon l'une des revendications précédentes, caractérisé en ce que la deuxième couche métallique (20) est produite par métallisation autocatalytique à l'aide de cuivre et/ou de nickel.
  7. Procédé selon l'une des revendications précédentes, caractérisé en ce que, entre la deuxième couche métallique (20) et la troisième couche (30), on dépose également une couche intermédiaire métallique de lissage (25).
  8. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'on dépose comme troisième couche (30) une troisième couche décorative.
  9. Procédé selon la revendication 8, caractérisé en ce que, pour la troisième couche décorative (30), on dépose du chrome, en particulier par voie galvanique.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'on utilise pour la troisième couche (30) un matériau ayant des propriétés anti-friction et/ou anti-usure.
  11. Système de couches obtenu par un procédé selon l'une des revendications précédentes.
  12. Système de couches présentant :
    un substrat (5) en métal léger ou en alliage léger,
    sur ce substrat, une première couche non conductrice (10) composée d'un oxyde du matériau du substrat,
    sur cette première couche, une deuxième couche (20) déposée par voie autocatalytique et composée d'un ou plusieurs métaux,
    une troisième couche (30).
  13. Système de couches selon la revendication 12, présentant en plus, entre la deuxième couche (20) et la troisième couche (30), une couche intermédiaire métallique de lissage (25).
  14. Système de couches selon la revendication 12 ou la revendication 13, caractérisé en ce que le substrat (5) se compose d'aluminium ou de magnésium ou d'un alliage à base d'aluminium ou de magnésium.
  15. Système de couches selon l'une des revendications 12 à 14, caractérisé en ce que la première couche non conductrice (10) a une épaisseur de 1 µm à 200 µm.
  16. Système de couches selon l'une des revendications 12 à 15, caractérisé en ce que la deuxième couche (20) déposée par voie autocatalytique a une épaisseur de 0,5 µm à 20 µm.
  17. Système de couches selon l'une des revendications 12 à 16, caractérisé en ce que la couche intermédiaire métallique (25) a une épaisseur de 2 µm à 20 µm.
  18. Jante ou jante décorative en métal léger, en particulier pour des véhicules automobiles, revêtue par l'un des procédés selon les revendications 1 à 10 ou munie d'un système de couches selon l'une des revendications 11 à 17.
EP99911717A 1998-02-26 1999-02-26 Procede pour produire un revetement de protection contre la corrosion et systeme en couches pour substrats en metal leger Expired - Lifetime EP1060291B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19807823A DE19807823A1 (de) 1998-02-26 1998-02-26 Verfahren zur Herstellung einer korrosionsschützenden Beschichtung und Schichtsystem für Substrate aus Leichtmetall
DE19807823 1998-02-26
PCT/EP1999/001267 WO1999043869A2 (fr) 1998-02-26 1999-02-26 Procede pour produire un revetement de protection contre la corrosion et systeme en couches pour substrats en metal leger

Publications (2)

Publication Number Publication Date
EP1060291A2 EP1060291A2 (fr) 2000-12-20
EP1060291B1 true EP1060291B1 (fr) 2001-12-19

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Family Applications (1)

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EP99911717A Expired - Lifetime EP1060291B1 (fr) 1998-02-26 1999-02-26 Procede pour produire un revetement de protection contre la corrosion et systeme en couches pour substrats en metal leger

Country Status (5)

Country Link
US (1) US6703135B1 (fr)
EP (1) EP1060291B1 (fr)
JP (1) JP4567187B2 (fr)
DE (2) DE19807823A1 (fr)
WO (1) WO1999043869A2 (fr)

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US8124240B2 (en) * 2005-06-17 2012-02-28 Tohoku University Protective film structure of metal member, metal component employing protective film structure, and equipment for producing semiconductor or flat-plate display employing protective film structure
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CN102724840B (zh) * 2011-03-29 2015-03-04 富准精密工业(深圳)有限公司 壳体及其制造方法
EP3421646A1 (fr) * 2017-06-29 2019-01-02 EMPA Eidgenössische Materialprüfungs- und Forschungsanstalt Procédé de coloration d'un élément en alliage d'aluminium

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015105139B4 (de) * 2014-04-08 2025-03-27 GM Global Technology Operations LLC (n. d. Gesetzen des Staates Delaware) Leichtmetallwerkstück und Verfahren zum Herstellen einer korrosionsbeständigen und glänzend erscheinenden Beschichtung für ein Leichtmetallwerkstück

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JP2002505379A (ja) 2002-02-19
WO1999043869A3 (fr) 1999-12-29
WO1999043869A2 (fr) 1999-09-02
DE59900592D1 (de) 2002-01-31
JP4567187B2 (ja) 2010-10-20
EP1060291A2 (fr) 2000-12-20
US6703135B1 (en) 2004-03-09
DE19807823A1 (de) 1999-09-09

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