EP0279146B1 - Procédé de coloration électrolytique d'une couche d'oxyde anodique sur l'aluminium ou un alliage de l'aluminium - Google Patents

Procédé de coloration électrolytique d'une couche d'oxyde anodique sur l'aluminium ou un alliage de l'aluminium Download PDF

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Publication number
EP0279146B1
EP0279146B1 EP87810782A EP87810782A EP0279146B1 EP 0279146 B1 EP0279146 B1 EP 0279146B1 EP 87810782 A EP87810782 A EP 87810782A EP 87810782 A EP87810782 A EP 87810782A EP 0279146 B1 EP0279146 B1 EP 0279146B1
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EP
European Patent Office
Prior art keywords
oxide layer
colouring
carried out
alternating current
process according
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
EP87810782A
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German (de)
English (en)
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EP0279146A1 (fr
Inventor
Jean-François Paulet
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.)
3A Composites International AG
Original Assignee
Alusuisse Lonza Services Ltd
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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
    • 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
    • C25D11/20—Electrolytic after-treatment
    • C25D11/22—Electrolytic after-treatment for colouring layers
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S204/00—Chemistry: electrical and wave energy
    • Y10S204/08—AC plus DC
    • 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
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S204/00—Chemistry: electrical and wave energy
    • Y10S204/09—Wave forms

Definitions

  • the invention relates to a method for electrolytic coloring of an anodic oxide layer on aluminum or aluminum alloys according to the preamble of claim 1.
  • this (s) is first anodically oxidized to form an oxide layer and then, in the case of unsealed pores in the oxide layer, of an electrolysis in an electrolytic solution which contains at least one metal salt, e.g. contains a nickel salt, which is colored by the electrodeposition of metal or metal oxide in the pores of the applied oxide layer.
  • at least one metal salt e.g. contains a nickel salt
  • the staining method described is used routinely and generally does not pose any problems if an extremely uniform staining is not necessary.
  • the colored coverings produced frequently show deviations in color, particularly in the case of irregularly shaped workpieces which have protruding or recessed parts.
  • Another disadvantage is that the uniformity and the speed of coloring decrease if a longer time elapses between the anodic treatment of the metal and the coloring or if the metal is rinsed off too long after the anodic treatment.
  • the dyeing process used in practice essentially takes place in such a way that the aluminum or the aluminum alloys are first anodized to form an oxide layer and the oxide layer thus formed is rinsed off with water. While the pores in this oxide layer are still unsealed, the anodized metal is immersed in an electrolyte solution together with a counter electrode. Before the electrolytic staining takes place in this solution, a direct current is passed through the solution, the anodically oxidized metal in the solution being connected anodically. The metal is then subjected to electrolysis in the same electrolyte, usually with alternating current, during which the coloring takes place.
  • a process of the type mentioned at the outset is known as known from GB-A-2 053 972 and EP-A-239 944 (prior art according to Art. 54 (3) and (4) EPC), the anodic pretreatment including undulating alternating current is carried out. From the abstract for JP-A-55 65 394, a one-step dyeing process with a rectangular alternating current is also known.
  • the invention has for its object to achieve a better uniformity of color and an increased dyeing speed in the electrolytic dyeing of anodic oxide layers on aluminum or aluminum alloys.
  • the object is achieved by a method which is distinguished by the wording of claim 1.
  • Advantageous further developments of the method according to the invention are characterized by the features of claims 2 to 9.
  • the coloring can take place by means of direct current, alternating current or asymmetrical alternating current.
  • the dyeing speed has a decisive influence on the corrosion resistance of the anodic evoked oxide coating.
  • the oxide layer is partially attacked, especially for darker shades where longer dyeing times - up to 10 minutes - are required.
  • Such layers are very susceptible to corrosion in later use and quickly show unaesthetic deposits when weathered.
  • a major advantage of the method according to the invention is that such disadvantages do not occur, especially when using a tin-containing electrolyte. Because of the resulting high dyeing speed, the dyeing time can be reduced and the attack of the oxide layer by the electrolyte can be virtually prevented, which benefits the corrosion resistance of the colored layer.
  • the metal is usually first degreased, rinsed with water or subjected to another suitable cleaning pretreatment. Then the pretreated metal in the electrolytic solution, which is usually acidic and sulfuric acid, oxalic acid, sulfamic acid or the like. contains, anodically connected, whereupon an electrical current is passed between the metal acting as the anode and a cathode also immersed in the solution.
  • the electrolytic solution which is usually acidic and sulfuric acid, oxalic acid, sulfamic acid or the like. contains, anodically connected, whereupon an electrical current is passed between the metal acting as the anode and a cathode also immersed in the solution.
  • the anodically oxidized metal is then subjected to electrolysis in a two-stage process, it being possible for both process steps to be carried out in the same electrolyte.
  • the first process step of the electrolysis is carried out according to the invention by passing an asymmetrical, rectangular alternating current through the electrolytic solution in which the anodic oxide layer is anodically connected. It works with a maximum voltage of about 10 to 30 volts. The best results were obtained at a voltage of 10 to 20 volts. It is advantageous not to carry out the first method step for longer than 5 minutes, preferably over a period of 5 to 60 seconds.
  • the second process step is basically known.
  • the anodically produced oxide layer can be independent of the duration of the rinsing are colored very evenly after their production. It was found that the coloring progresses very quickly when the anodized metal is treated in the pretreatment process according to the invention with a voltage of the asymmetrical, rectangular alternating current which is lower or similar to that which is used for the subsequent coloring process.
  • the color depth and the uniformity of the coloring were determined on the basis of reflection measurements: the higher the color depth, the lower the reflection value R and, for measurements at different locations on the sample sheet to be colored, the more uniform the coloring, the lower the difference in reflection value ⁇ R.
  • An electrolyte containing 100 g / l NiSO4.6 H2O, 40 g / l boric acid and sulfuric acid was used at a pH of 4.0.
  • the bathroom was in a rectangular container with a side length of 60 and 130 cm.
  • graphite electrodes at a distance of 6 cm from the wall as counter electrodes to the aluminum alloy sheet to be colored.
  • the area ratio of the counterelectrode and the sheet to be colored was 1. The sheet was placed in the middle of the container so that all the electrodes were at an even distance from it.
  • the current voltages were the maximum voltages in the positive and negative range, ie amplitude positive V+ and amplitude negative V+, and the duration of the current in the positive and negative part, measured in milliseconds and designated as mS+ and mS ⁇ , respectively constant dyeing time varied from 2 minutes.
  • the coloring effect was followed on the basis of reflection measurements with the Unigalvo device.
  • the Calibration was done with standard white, which was set to reflectivity of 80%.
  • the reflection measurements were carried out in the middle and the diagonally opposite corner areas.
  • the reflection values determined show that, in comparison with the corresponding comparison tests, the reflection value difference ⁇ R is always lower in the tests using the method according to the invention, which means that in the tests carried out according to the invention the sheet was colored more uniformly than in the conventional ones Process colored sheets, and the reflection values themselves are always lower, which means that the color intensity or depth of color is stronger in the sheets colored by the inventive method than in the conventionally colored.
  • the process according to the invention identifies the latter as the one with the faster dyeing speed.
  • Example 2 In a manner analogous to that in Example 1, a test series consisting of 7 tests was carried out, the test conditions and results being summarized in Table 2.
  • the bath container was the same as in Example 1.
  • the test sheets to be colored consisted of the Almg1 alloy, had a size of 10 ⁇ 25 cm and were provided with an anodically (direct current) oxidized layer 20 ⁇ m.
  • a single graphite counter electrode was used in one corner of the container.
  • the sample plates were arranged parallel to the longer wall of the container at a distance of 8 cm.
  • the area ratio of the counter electrode to the sheet was 0.1. 5 reflection measurements were carried out at regular intervals over the length of the sheet, the reflection value 1 being the measured value in the sheet metal area opposite the counterelectrode and reflection value 5 the measured value being the most distant sheet metal area of the counterelectrode.

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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)

Claims (9)

  1. Procédé pour la coloration électrolytique d'une couche d'oxyde anodique sur l'aluminium ou des alliages d'aluminium au moyen de courant continu ou de courant alternatif dans un électrolyte contenant au moins un sel métallique, dans lequel avant la coloration de la couche d'oxyde, celle-ci est prétraitée, branchée en anode, par un courant alternatif asymétrique, dont l'amplitude de la portion de tension négative est inférieure ou égale à celle de la portion de tension positive, caractérisé en ce que le prétraitement est mis en oeuvre avec un courant alternatif rectangulaire.
  2. Procédé selon la revendication 1, caractérisé en ce que la couche d'oxyde est prétraitée dans le même électrolyte que celui dans lequel s'effectue la coloration ultérieure.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que l'amplitude de la portion de tension positive est de 10 à 30 V, de préférence de 10 à 20 V.
  4. Procédé selon les revendications 1 à 3, caractérisé en ce que la couche d'oxyde est prétraitée pendant au maximum 5 min, de préférence de 5 à 60 s.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la coloration s'effectue en courant continu.
  6. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que la coloration s'effectue en courant alternatif.
  7. Procédé selon la revendication 6, caractérisé en ce que la coloration s'effectue en courant alternatif asymétrique.
  8. Procédé selon l'une des revendications 5 à 7, caractérisé en ce que la coloration s'effectue avec une tension maximale d'environ 8 à 40 V, de préférence à environ 10 à 30 V.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce que l'on utilise un électrolyte contenant de l'étain.
EP87810782A 1987-01-16 1987-12-24 Procédé de coloration électrolytique d'une couche d'oxyde anodique sur l'aluminium ou un alliage de l'aluminium Expired - Lifetime EP0279146B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH145/87 1987-01-16
CH14587 1987-01-16

Publications (2)

Publication Number Publication Date
EP0279146A1 EP0279146A1 (fr) 1988-08-24
EP0279146B1 true EP0279146B1 (fr) 1992-03-25

Family

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EP87810782A Expired - Lifetime EP0279146B1 (fr) 1987-01-16 1987-12-24 Procédé de coloration électrolytique d'une couche d'oxyde anodique sur l'aluminium ou un alliage de l'aluminium

Country Status (3)

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US (1) US4798656A (fr)
EP (1) EP0279146B1 (fr)
DE (1) DE3777806D1 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3743113A1 (de) * 1987-12-18 1989-06-29 Gartner & Co J Verfahren zum elektrolytischen faerben von anodisch erzeugten oxidschichten auf aluminium und aluminiumlegierungen
US4931151A (en) * 1989-04-11 1990-06-05 Novamax Technologies Holdings Inc. Method for two step electrolytic coloring of anodized aluminum
JPH02301596A (ja) * 1989-05-16 1990-12-13 Minoru Mitani アルミニウム又はその合金の表面処理方法
US5674371A (en) * 1989-11-08 1997-10-07 Clariant Finance (Bvi) Limited Process for electrolytically treating aluminum and compositions therefor
EP0487754A1 (fr) * 1990-11-25 1992-06-03 BEFELD SYSTEME GmbH Procédé de coloration électrolytique de couches d'oxyde obtenues par voie anodique sur l'aluminium et d'alliages de l'aluminium
ES2052455B1 (es) * 1992-12-31 1994-12-01 Novamax Tech Holdings Procedimiento para la obtencion por via electrolitica sobre aluminio anodizado de una gama de colores del espectro visible.
US6113770A (en) * 1997-09-18 2000-09-05 Pioneer Metal Finishing Corporation Method for anodizing using single polarity pulses
JP5207124B2 (ja) * 2008-03-24 2013-06-12 スズキ株式会社 陽極酸化処理方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0239944A1 (fr) * 1986-04-01 1987-10-07 Fujisash Company Procédé d'électrocoloration d'aluminium ou d'alliages d'aluminium

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US31901A (en) * 1861-04-02 Improved refrigerator
JPS5652116B2 (fr) * 1973-03-09 1981-12-10
US3989605A (en) * 1973-03-09 1976-11-02 Sumitomo Chemical Company, Limited Method for continuous electrolytic coloring of aluminum articles
JPS5334107B2 (fr) 1974-04-23 1978-09-19
NO762506L (fr) * 1975-07-24 1977-01-25 Sumitomo Chemical Co
ES8205885A2 (es) * 1979-07-04 1982-08-01 Empresa Nacional Aluminio Mejoras introducidas en el objeto de la patente principal por proceso para la coloracion electrolitica del aluminio a-nodizado.

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0239944A1 (fr) * 1986-04-01 1987-10-07 Fujisash Company Procédé d'électrocoloration d'aluminium ou d'alliages d'aluminium

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Publication number Publication date
EP0279146A1 (fr) 1988-08-24
US4798656A (en) 1989-01-17
DE3777806D1 (de) 1992-04-30

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