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EP1678345B1 - Couches de conversion colorees sans chrome formees sur des surfaces metalliques - Google Patents

Couches de conversion colorees sans chrome formees sur des surfaces metalliques Download PDF

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Publication number
EP1678345B1
EP1678345B1 EP04790238.2A EP04790238A EP1678345B1 EP 1678345 B1 EP1678345 B1 EP 1678345B1 EP 04790238 A EP04790238 A EP 04790238A EP 1678345 B1 EP1678345 B1 EP 1678345B1
Authority
EP
European Patent Office
Prior art keywords
ions
treatment solution
aqueous treatment
metal
persulfate
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
EP04790238.2A
Other languages
German (de)
English (en)
Other versions
EP1678345A1 (fr
Inventor
Pavel Gentschev
Matthias Schweinsberg
Marco Bastian
Ulrich JÜPTNER
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP1678345A1 publication Critical patent/EP1678345A1/fr
Application granted granted Critical
Publication of EP1678345B1 publication Critical patent/EP1678345B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • C23C22/66—Treatment of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process

Definitions

  • the invention is in the field of chemical surface treatment of zinc or galvanized steel, aluminum, magnesium or their alloys. It describes chromium-free conversion processes for such metal surfaces, i. H. chemical treatment processes which result in the formation of a surface layer in which both cations of the treated metal surface and ions from the treatment solution are incorporated.
  • the chromium-free coating is colored, so that it can be determined by simple visual inspection whether a sufficient conversion layer has been formed.
  • the object of this conversion layer is to reduce the tendency of the metal surface to corrode and to produce good adhesion between the metal surface and an organic coating such as a lacquer or an adhesive applied to the conversion layer.
  • WO 94/25640 a method of producing blue colored conversion coatings on zinc / aluminum alloys.
  • the metal surfaces are brought into contact with a treatment solution which has a pH of between 3.5 and 6 and contains 0.2 to 3.0% by weight of molybdenum and a fluoride content of 0.1 to 2.0% by weight. % having.
  • Molybdenum can be used as molybdate, as phosphomolybdic acid, as molybdenum chloride and the like.
  • Fluoride can be used in the form of hydrofluoric acid, simple fluorides, but also complex fluoro acids such as fluorotitanic acid or fluorozirconic acid.
  • the treatment solution contains heterooxoanions of molybdenum, tungsten or vanadium with one of the heteroions phosphorus, aluminum, silicon, manganese, zirconium, titanium, tin, cerium or nickel.
  • the treatment solution contains an organic film former, which can be selected for example from acrylates.
  • the heterooxo anions such as, for example, anions of heteropolyacids, can be formed directly in the treatment solution by adding thereto the starting materials, for example molybdate ions and phosphoric acid.
  • the treatment solution should preferably contain an etchant for aluminum, for example fluoride, tetrafluoroborate or similar etchant.
  • the doctrine of WO 00/26437 goes the way to colorize the conversion layer by an organic dye (Alizerinfarbstoff).
  • the conversion layer itself is produced with a treatment solution which contains complex fluorides, for example of titanium and zirconium, in addition to further inorganic oxides, hydroxides or carbonates or their reaction products with the fluoro acids.
  • a treatment solution which contains complex fluorides, for example of titanium and zirconium, in addition to further inorganic oxides, hydroxides or carbonates or their reaction products with the fluoro acids.
  • an amino-substituted poly-4-hydroxy-styrene polyvinylphenol
  • colored layers on aluminum can be obtained by chemical oxidation with aromatic nitro compounds.
  • the different positional isomers of nitrobenzoic acid can be used for this purpose.
  • the chemical oxidation of aluminum surfaces with persulfate ions is reported in DE-A-741 337 described.
  • the aim is to produce crystal-clear and colorless layers on aluminum and its alloys.
  • such layers are obtained by allowing ammonia to act on the carefully cleaned light metal in a hot, aqueous solution which also contains an addition of alkali persulfate, suitably 1%.
  • the cleaning can be done for example by immersion in concentrated nitric acid.
  • the treatment with the ammoniacal persulfate solution takes place at temperatures of at least 70 ° C.
  • the duration is about 15 to 60 minutes. It is reported that at temperatures below 70 ° C also receives protective layers, but are less transparent and often yellowish. In the context of the disclosure of said document such yellowish layers are apparently undesirable, since one does not want to paint the treated parts, but to retain their metallic appearance.
  • the inventors of the present invention have found that reduced (light gold to golden) layers on surfaces of suitable metals obtained at reduced temperature and reduced treatment time, on the one hand chromium-free and on the other hand excellent adhesion to a subsequently applied coating based organic polymers, for example a paint or an adhesive.
  • the object of the present invention is now to maintain the effectiveness of such treatment methods of surfaces of zinc, aluminum, magnesium or their alloys for a prolonged period of time.
  • the present invention relates, in a first aspect, to a process for producing colored layers on surfaces of zinc, aluminum, magnesium or their alloys by contacting the surfaces with a chromium-free aqueous treatment solution containing a total of 3 to 35 g / l of persulfate ions and / or or peroxodisulfate ions, in addition from about 1 to about 50 g / l sulfate ions and not more than 10 g / l ammonia or ammonium ions, has a pH in the range of 10 to 12 and a temperature in the range of 30 to 70 ° C, wherein the surfaces for a period in the range of 0.5 to 5 minutes with the Contact treatment solution.
  • the treatment solution may contain 8 to 35 g / L of persulfate ions.
  • the persulfate and / or peroxodisulfate ions are preferably introduced into the treatment solution as alkali metal salts, in particular as sodium or potassium salt.
  • the sulfate ions are introduced, for example, in the form of sodium or potassium salts.
  • the excess of sulfate ions means that to maintain the required alkaline pH in the course of the process according to the invention less sodium hydroxide must be added than without this excess. This saves on chemicals costs.
  • the required alkaline pH is preferably adjusted by an alkali metal hydroxide solution, in particular by sodium hydroxide solution and / or potassium hydroxide solution.
  • the aqueous treatment solution does not contain more than 1 g / L of ammonia or ammonium ions.
  • the treatment solution in the process of the invention has a temperature in the range of 30 to 70 ° C.
  • the treatment time is in the range of 0.5 to 5 minutes. At lower treatment times, sufficient layers are no longer formed. Although treatment times of more than 5 minutes lead to strongly colored layers, the paint adhesion on these layers deteriorates.
  • the surfaces are first cleaned prior to the chemical oxidation step. This can be done for example by brief pickling in cold, concentrated nitric acid. Or the surfaces are rubbed with a chamois leather.
  • an alkaline cleaning solution if desired with water, preferably with deionized water Water, rinsed and then in an acidic solution, for example in nitric acid, dekapiert.
  • the metal surfaces are prepared so that they assume a uniform light golden to golden coloration on the one hand in the process step of chemical oxidation and on the other hand have good adhesion properties to a subsequent coating based on organic polymers.
  • sulfate ions for example in the form of sodium or potassium salts, brings about the same technical effect as described in the process according to the invention for producing colored layers and thus solves the problem underlying the invention.
  • the metal surfaces are rinsed with water, preferably with demineralized water.
  • the metal surfaces are dried after rinsing with water or not. If the coating with organic polymers, for example, in such a way that immersing the metal surfaces in an aqueous coating dispersion, a drying after rinsing is not required. However, if the organic polymer-based coating is, for example, an adhesive or a powder coating, it is preferable to dry the metal surfaces prior to this step.
  • the invention relates to a method according to one or more of claims 1 to 5, characterized in that the metal surfaces, after it has been brought into contact with the aqueous treatment solution, rinsed and coated with a coating based on organic polymers.
  • these metal strips, metal sheets or metal parts on the colored conversion layer which results from the treatment with the persulfate and / or peroxodisulfate-containing solution, carry a coating based on organic polymers, for example one or more paint layers or an adhesive layer.
  • the metal parts according to the invention can be connected to other metal parts.
  • the painted test panels were subjected to a cross-hatch cooking test to test the paint adhesion.
  • corrosion test salt spray test according to DIN 50021 SS was carried out and the paint infiltration at the Ritz was measured according to DIN 53167. The results are included in Table 1.
  • Table 1 Treatment parameters and treatment results Experiment No.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Paints Or Removers (AREA)

Claims (6)

  1. Procédé pour l'obtention de couches colorées sur des surfaces de zinc, d'aluminium, de magnésium ou de leurs alliages, dans lequel on met les surfaces en contact avec une solution de traitement aqueuse exempte de chrome, qui contient au total de 3 à 35 g/litre d'ions de persulfate et/ou d'ions de peroxodisulfate et pas plus de 10 g/l d'ammoniac ou d'ions ammonium, et qui présente une valeur de pH dans la plage de 10 à 12 et une température dans la plage de 30 à 70 °C, dans lequel on met les surfaces en contact avec la solution de traitement pendant un laps de temps dans la plage de 0,5 à 5 minutes, caractérisé en ce que la solution de traitement aqueuse contient en outre de 1 à 50 g/l d'ions de sulfate.
  2. Procédé selon la revendication 1, caractérisé en ce que la solution de traitement contient de 8 à 35 g/litre d'ions de persulfate.
  3. Procédé selon une des revendications précédentes ou les deux, caractérisé en ce qu'on introduit les ions de persulfate et/ou de peroxodisulfate sous la forme de sels de métaux alcalins et en ce qu'on règle la valeur de pH de la solution de traitement aqueuse avec de la lessive de soude et/ou de la lessive potassique.
  4. Procédé selon une ou plusieurs des revendications 1 à 3, caractérisé en ce que la solution de traitement aqueuse ne contient pas plus de 1 g/l d'ammoniac ou d'ions ammonium.
  5. Procédé selon une ou plusieurs des revendications 1 à 4, caractérisé en ce que la solution de traitement aqueuse ne contient pas d'autres ions métalliques à titre d'ions de métaux alcalins et/ou d'ions alcalino-terreux.
  6. Procédé selon une ou plusieurs des revendications 1 à 5, caractérisé en ce qu'après avoir mis les surfaces métalliques en contact avec la solution de traitement aqueuse, on les rince et on les recouvre d'une enduction à base de polymères organiques.
EP04790238.2A 2003-11-07 2004-10-09 Couches de conversion colorees sans chrome formees sur des surfaces metalliques Expired - Lifetime EP1678345B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10352076 2003-11-07
PCT/EP2004/011315 WO2005047565A1 (fr) 2003-11-07 2004-10-09 Couches de conversion colorees sans chrome formees sur des surfaces metalliques

Publications (2)

Publication Number Publication Date
EP1678345A1 EP1678345A1 (fr) 2006-07-12
EP1678345B1 true EP1678345B1 (fr) 2013-11-20

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP04790238.2A Expired - Lifetime EP1678345B1 (fr) 2003-11-07 2004-10-09 Couches de conversion colorees sans chrome formees sur des surfaces metalliques

Country Status (3)

Country Link
US (2) US7828911B2 (fr)
EP (1) EP1678345B1 (fr)
WO (1) WO2005047565A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10287665B2 (en) 2014-06-27 2019-05-14 Henkel Ag & Co. Kgaa Dry lubricant for zinc coated steel

Families Citing this family (7)

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Publication number Priority date Publication date Assignee Title
US7413777B2 (en) * 2004-06-12 2008-08-19 Allfast Fastening Systems, Inc. Coating composition and methods of coating
US8461631B2 (en) * 2007-02-23 2013-06-11 Sensor Electronic Technology, Inc. Composite contact for semiconductor device
US8338871B2 (en) * 2008-12-23 2012-12-25 Sensor Electronic Technology, Inc. Field effect transistor with electric field and space-charge control contact
US8586997B2 (en) 2011-02-15 2013-11-19 Sensor Electronic Technology, Inc. Semiconductor device with low-conducting field-controlling element
WO2013036593A1 (fr) 2011-09-06 2013-03-14 Sensor Electronic Technology, Inc. Dispositif à semi-conducteur doté d'un élément de commande de champ à faible conduction
US8994035B2 (en) 2011-11-21 2015-03-31 Sensor Electronic Technology, Inc. Semiconductor device with low-conducting buried and/or surface layers
US9673285B2 (en) 2011-11-21 2017-06-06 Sensor Electronic Technology, Inc. Semiconductor device with low-conducting buried and/or surface layers

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DE4317217A1 (de) * 1993-05-24 1994-12-01 Henkel Kgaa Chromfreie Konversionsbehandlung von Aluminium
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10287665B2 (en) 2014-06-27 2019-05-14 Henkel Ag & Co. Kgaa Dry lubricant for zinc coated steel

Also Published As

Publication number Publication date
US7828911B2 (en) 2010-11-09
WO2005047565A1 (fr) 2005-05-26
US20060272748A1 (en) 2006-12-07
US20110011498A1 (en) 2011-01-20
US8268096B2 (en) 2012-09-18
EP1678345A1 (fr) 2006-07-12

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