EP0459550B1 - Procédé de rinçage de couches de conversion - Google Patents

Procédé de rinçage de couches de conversion Download PDF

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Publication number
EP0459550B1
EP0459550B1 EP91201021A EP91201021A EP0459550B1 EP 0459550 B1 EP0459550 B1 EP 0459550B1 EP 91201021 A EP91201021 A EP 91201021A EP 91201021 A EP91201021 A EP 91201021A EP 0459550 B1 EP0459550 B1 EP 0459550B1
Authority
EP
European Patent Office
Prior art keywords
solutions
rinsed
process according
conversion coatings
rinsing
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
EP91201021A
Other languages
German (de)
English (en)
Other versions
EP0459550A1 (fr
Inventor
Thomas Kolberg
Werner Dr. Rausch
Peter Dr. Schubach
Thomas Wendel
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.)
Chemetall GmbH
Original Assignee
Metallgesellschaft AG
Continentale Parker Ste
Continentale Parker SA
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 Metallgesellschaft AG, Continentale Parker Ste, Continentale Parker SA filed Critical Metallgesellschaft AG
Publication of EP0459550A1 publication Critical patent/EP0459550A1/fr
Application granted granted Critical
Publication of EP0459550B1 publication Critical patent/EP0459550B1/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
    • C23C22/06—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 aqueous acidic solutions with pH less than 6
    • C23C22/34—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 aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • 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
    • C23C22/06—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 aqueous acidic solutions with pH less than 6
    • C23C22/34—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 aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—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 aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/361—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 aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing titanium, zirconium or hafnium compounds
    • 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
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment

Definitions

  • the invention relates to a method for rinsing conversion surfaces produced on surfaces made of aluminum or aluminum alloys with chromium-free solutions based on complex fluorides of titanium, zirconium and / or hafnium, and its use as a pretreatment for subsequent painting, film coating or adhesive coating.
  • conversion layers on aluminum or aluminum alloy surfaces in particular as pretreatment before the application of an organic coating, is carried out industrially on a large scale.
  • Conversion layers of this type prevent or make it more difficult for corrosion to occur and, in the case of an organic coating, serve to improve the adhesion of the applied coating.
  • the widespread chromate coatings generally meet these requirements to a sufficient extent; for reasons of workplace hygiene, environmental protection or because the treated material for special purposes, e.g. As food packaging, however, the generation of chrome-free conversion layers is increasingly preferred.
  • the treatment solutions used for this are generally adjusted to an acidic pH and contain e.g. Titanium, fluoride, phosphate and tannin (U.S. Patent 4,017,334) or zirconium, fluoride and boron (U.S. Patent 3,964,936).
  • a treatment solution containing hafnium and fluoride is described in FR-PS 2 417 537.
  • the properties of the conversion layers generated can be further improved if a passivating rinsing is subsequently carried out.
  • Chromium-free treatment solutions are also preferred for rinsing, which usually contain organic active ingredients.
  • Such a rinse aid based on polyvinylphenol is described in US-A 4,376,000. However, it causes a pollution of the wastewater, in particular due to the high oxygen demand, which is necessary to break down the organic component.
  • the object of the invention is to provide a method for passivating rinsing of chrome-free conversion layers produced on surfaces made of aluminum or aluminum alloys with solutions based on complex fluorides of titanium, zirconium and / or hafnium, which does not have the disadvantage of rinsing solutions with organic components with regard to waste water treatment has, but improves the corrosion protection and paint adhesion in at least the same way.
  • the object is achieved by designing the method of the type mentioned at the outset in accordance with the invention in such a way that the conversion layers are rinsed with aqueous solutions which contain aluminum, zirconium and fluoride with a molar ratio of Al: Zr: F of (0, 15 to 2.0): 1: (5 to 16), and whose pH is adjusted to 2 to 5.
  • the method according to the invention is suitable for the passivating rinsing of conversion layers which have been produced on aluminum or aluminum alloy surfaces, wherein the materials can consist of solid aluminum or solid aluminum alloy or objects plated therewith, for example, in the hot-dip method.
  • the material can be made of steel, which has been provided with an aluminum or aluminum alloy surface using the hot-dip process.
  • Suitable alloying partners for aluminum are in particular silicon, manganese, magnesium, zinc and copper.
  • the conversion layers produced on such surfaces with solutions based on Ti, Zr and / or Hf are distinguished by the fact that the layer thickness is clearly below 1 ⁇ m, the layers are at least partially amorphous and that they contain no chromium.
  • the treatment solutions by means of which the conversion layers are produced contain, in addition to titanium, zirconium and / or hafnium ions, further layer-forming and / or pickling components, such as e.g. Fluorides, phosphates, compounds of boron, and possibly passivating components such as Tannins. Suitable treatment solutions are described in the patents mentioned at the beginning.
  • the surface is expediently rinsed with water after the conversion layer has been produced.
  • the application of the rinse solution can e.g. by dipping, flooding, spraying or rolling.
  • a preferred embodiment of the invention consists in rinsing with a solution which contains aluminum, zirconium and fluoride in a total concentration Al + Zr + F between 0.1 and 8 g / l, preferably between 0.2 and 5 g / l.
  • the Al: Zr: F molar ratios should advantageously be set to (0.15 to 0.67): 1: (5 to 7).
  • the rinse solutions used in the method according to the invention contain, inter alia, acidic aluminum fluorozirconates and, in the case of an excess of aluminum, other salts of aluminum (e.g. fluorides, tetrafluoroborates, nitrates).
  • Their manufacture can e.g. in such a way that metallic zirconium or zirconium carbonate is first dissolved in aqueous hydrofluoric acid, complex fluorozirconic acid being formed. Then metallic aluminum or aluminum hydroxide or an aluminum salt, e.g. Nitrate, fluoride, tetrafluoroborate, formate, acetate, preferably in dissolved form, are added and, if necessary, dissolved. A possible slight clouding of the solution does not affect the effectiveness.
  • the solutions can also be prepared in other ways.
  • the pH of the solution is preferably adjusted with cations of volatile bases. These include in particular ammonium, ethanolammonium and di- and tri-ethanolammonium.
  • volatile bases include in particular ammonium, ethanolammonium and di- and tri-ethanolammonium.
  • the surfaces provided with a conversion coating are rinsed with an aqueous solution which additionally contain at least one of the anions benzoate, caprylate, ethylhexoate, salicylate in a total concentration of preferably 0.05 to 0.5 g / l.
  • anions can be introduced via the corresponding acids or their salts.
  • the duration of the application of the rinse solution is generally between about 1 and 120 seconds, according to an expedient embodiment of the invention between 1 and 30 seconds.
  • the application temperature can be between 20 ° C and about 80 ° C. Temperatures between 20 and 50 ° C are preferred.
  • Demineralized or low-salt water is preferably used for the preparation of the rinse bath. Water with a high salt content is less suitable for bath preparation.
  • the surface can e.g. air-dried or oven-dried, if necessary rinsed with deionized water beforehand.
  • An advantageous embodiment of the invention provides that the surface is accelerated after the passivative rinsing, e.g. dry with hot air or infrared radiation.
  • the method according to the invention is primarily used to pretreat the aluminum or aluminum alloy surfaces before painting, film coating or applying adhesives.
  • organic coating agents used are polyesters, silicone-modified polyesters, polyvinylidene fluorides, acrylates, epoxies, epoxy-phenol resins, plastisols or organosols (e.g. PVC or acrylates).
  • the advantage of the method according to the invention lies in particular in the increase in the adhesion of the organic films to the metallic substrate, as is the case, for example, with correspondingly good results in the T-Bend test (ISO 1519-1973) or in the feathering test (paint adhesion when opening the can closures ) is expressed.
  • the durability of the organic films Corrosion stress, e.g. increased in a condensation water constant climate test (DIN 50 017 KK) or a sterilization test.
  • the method according to the invention improves the corrosion resistance of the non-organically coated surface, as can be seen, for example, in the test for fountain blackness (no blackening when boiling in water).
  • the sheets were then rinsed with water and, after passivation, rinsed. For this purpose, the sheets were immersed in the rinse solution for 5 seconds and then excess solution was removed by squeezing. After a drying time of 0.5 min in a convection oven at 60 ° C, the sheets were coated with a two-layer food lacquer, the first layer of which is an epoxy-phenol resin and the second layer of which is an organosol.
  • the layer thickness of the overall paint was between 10 and 15 ⁇ m.
  • the rinsing solution used was diluted 1.6 g / l (rinsing solution A) or 3.2 g / l (rinsing solution B) of an aqueous concentrate with 0.855 wt .-% Al and 8.62 wt .-% Zr and 10.7 wt% F made using deionized water.
  • the pH in both solutions had been adjusted to approximately 3.6 with ammonia.
  • composition of the rinse solutions used in the process according to the invention was:

Landscapes

  • 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)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Laminated Bodies (AREA)

Claims (12)

  1. Procédé de rinçage de couches de conversion exemptes de chrome produites sur des surfaces en aluminium ou en alliages d'aluminium, par des solutions à base de fluorures complexes du titane, du zirconium et/ou de l'hafnium, caractérisé en ce qu'il consiste à rincer des couches de conversion par des solutions aqueuses, qui ont une teneur en aluminium, en zirconium et en fluorure en un rapport molaire de Al : Zr : F de (0,15 à 2,0) : 1 : (5 à 16) et dont le pH est réglé entre 2 et 5.
  2. Procédé suivant la revendication 1, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions dont la concentration totale en Al + Zr + F est comprise entre 0,1 et 8,0 g/l.
  3. Procédé suivant la revendication 1 ou 2, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions dont la concentration totale en Al + Zr + F est comprise entre 0,2 et 5,0 g/l.
  4. Procédé suivant la revendication 1, 2 ou 3, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions dans lesquelles les rapports molaires Al : Zr : F sont réglés à (0,15 à 0,67) : 1 : (5 à 7).
  5. Procédé suivant l'une on plurieurs des revendications 1 à 4, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions dont le pH est réglé par des cations de bases volatiles.
  6. Procédé suivant la revendication 5, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions dont le pH est réglé par des composés d'ammonium, d'éthanolammonium, de diéthanolammonium ou de triéthanolammonium.
  7. Procédé suivant l'une ou plusieurs des revendications 1 à 6, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions qui contiennent en outre au moins l'un des anions benzoate, caprylate, éthylhexoate, salicylate en une concentration totale de 0,05 à 0,5 g/l.
  8. Procédé suivant l'une ou plusieurs des revendications 1 à 7, caractérisé en ce qu'il consiste à rincer les couches de conversion pendant 1 à 30 secondes.
  9. Procédé suivant l'une ou plusieurs des revendications 1 à 8, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions qui ont une température de 20 à 80°C.
  10. Procédé suivant la revendication 9, caractérisé en ce qu'il consiste à rincer les couches de conversion par des solutions ayant une température de 20 à 50°C.
  11. Procédé suivant l'une ou plusieurs des revendications 1 à 10, caractérisé en ce qu'il consiste à sécher la surface après le rinçage.
  12. Utilisation du procédé suivant l'une ou plusieurs des revendications 1 à 11 comme prétraitement pour un laquage un pelliplacage ou un revêtement par adhésif ultérieur.
EP91201021A 1990-05-29 1991-04-29 Procédé de rinçage de couches de conversion Expired - Lifetime EP0459550B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4017187 1990-05-29
DE4017187A DE4017187A1 (de) 1990-05-29 1990-05-29 Verfahren zur nachspuelung von konversionsschichten

Publications (2)

Publication Number Publication Date
EP0459550A1 EP0459550A1 (fr) 1991-12-04
EP0459550B1 true EP0459550B1 (fr) 1993-12-01

Family

ID=6407364

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91201021A Expired - Lifetime EP0459550B1 (fr) 1990-05-29 1991-04-29 Procédé de rinçage de couches de conversion

Country Status (8)

Country Link
EP (1) EP0459550B1 (fr)
JP (1) JP3083873B2 (fr)
AU (1) AU634652B2 (fr)
BR (1) BR9102174A (fr)
CA (1) CA2041891C (fr)
DE (2) DE4017187A1 (fr)
ES (1) ES2047370T3 (fr)
ZA (1) ZA914086B (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06322287A (ja) * 1993-05-14 1994-11-22 Nippon Parkerizing Co Ltd 表面処理された複合アルミニウムパウダー、およびそれを用いる表面処理された複合アルミニウムフレークの製造方法
DE4317217A1 (de) * 1993-05-24 1994-12-01 Henkel Kgaa Chromfreie Konversionsbehandlung von Aluminium
IT1273111B (it) * 1994-04-07 1997-07-04 Skf Ind Spa Procedimento di preassemblaggio di un anello magnetizzato multipolare, in particolare per l'applicazione in dispositivi di rilevamento della velocita' di rotazione, e prodotto relativo
WO1996021752A1 (fr) * 1995-01-10 1996-07-18 Circle-Prosco, Inc. Procede de revetements de surfaces metalliques, destine a produire une surface fortement hydrophile et fortement resistante a la corrosion, qui est bioresistante et qui degage peu d'odeurs
US7402214B2 (en) 2002-04-29 2008-07-22 Ppg Industries Ohio, Inc. Conversion coatings including alkaline earth metal fluoride complexes
US6749694B2 (en) 2002-04-29 2004-06-15 Ppg Industries Ohio, Inc. Conversion coatings including alkaline earth metal fluoride complexes
DE102016206418A1 (de) * 2016-04-15 2017-10-19 Henkel Ag & Co. Kgaa Unterdrückung anlagenbedingter phosphatüberschleppung in einer prozessfolge zur tauchlackierung
DE102016206417A1 (de) 2016-04-15 2017-10-19 Henkel Ag & Co. Kgaa Fördergestellbehandlung zur unterdrückung anlagenbedingter phosphatüberschleppung in einer prozessfolge zur tauchlackierung

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3850732A (en) * 1970-12-02 1974-11-26 Amchem Prod Zirconium rinse for phosphate coated metal surfaces
US3895970A (en) * 1973-06-11 1975-07-22 Pennwalt Corp Sealing rinse for phosphate coatings of metal
US3912548A (en) * 1973-07-13 1975-10-14 Amchem Prod Method for treating metal surfaces with compositions comprising zirconium and a polymer
US4462842A (en) * 1979-08-13 1984-07-31 Showa Aluminum Corporation Surface treatment process for imparting hydrophilic properties to aluminum articles
US4370177A (en) * 1980-07-03 1983-01-25 Amchem Products, Inc. Coating solution for metal surfaces
US4496404A (en) * 1984-05-18 1985-01-29 Parker Chemical Company Composition and process for treatment of ferrous substrates
DE3829154A1 (de) * 1988-08-27 1990-03-01 Collardin Gmbh Gerhard Chromfreies verfahren zur vorbehandlung von metallischen oberflaechen vor einer beschichtung mit organischen materialien
DE3924984A1 (de) * 1989-07-28 1991-01-31 Metallgesellschaft Ag Verfahren zur passivierenden nachspuelung von phosphatschichten

Also Published As

Publication number Publication date
AU634652B2 (en) 1993-02-25
CA2041891C (fr) 2001-07-31
ES2047370T3 (es) 1994-02-16
ZA914086B (en) 1993-01-27
AU7618091A (en) 1991-12-12
JPH04231480A (ja) 1992-08-20
DE59100650D1 (de) 1994-01-13
BR9102174A (pt) 1991-12-24
CA2041891A1 (fr) 1991-11-30
DE4017187A1 (de) 1991-12-05
JP3083873B2 (ja) 2000-09-04
EP0459550A1 (fr) 1991-12-04

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