EP1200641B1 - Traitement prealable de surfaces d'aluminium a l'aide de solutions exemptes de chrome - Google Patents

Traitement prealable de surfaces d'aluminium a l'aide de solutions exemptes de chrome Download PDF

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Publication number
EP1200641B1
EP1200641B1 EP00925252A EP00925252A EP1200641B1 EP 1200641 B1 EP1200641 B1 EP 1200641B1 EP 00925252 A EP00925252 A EP 00925252A EP 00925252 A EP00925252 A EP 00925252A EP 1200641 B1 EP1200641 B1 EP 1200641B1
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EP
European Patent Office
Prior art keywords
workpieces
treatment
application
optionally
free
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
EP00925252A
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German (de)
English (en)
Other versions
EP1200641A1 (fr
Inventor
Thomas Wendel
Klaus Bittner
Hardy Wietzoreck
Peter Müller
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.)
Bayerische Motoren Werke AG
Chemetall GmbH
Original Assignee
Bayerische Motoren Werke AG
Chemetall GmbH
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Publication date
Application filed by Bayerische Motoren Werke AG, Chemetall GmbH filed Critical Bayerische Motoren Werke AG
Publication of EP1200641A1 publication Critical patent/EP1200641A1/fr
Application granted granted Critical
Publication of EP1200641B1 publication Critical patent/EP1200641B1/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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals
    • C23G1/125—Light metals aluminium

Definitions

  • the invention relates to a method for the pretreatment of Workpieces with a surface of aluminum or Aluminum alloys for chipless forming and / or the bonding by welding or gluing with similar pretreated or otherwise otherwise precoated workpieces or optionally Pre-treated parts made of steel and / or galvanized and / or alloy-galvanized steel and for a subsequent anti-corrosive treatment by Phosphating, by a chromium-free conversion treatment, by primer application or by painting.
  • the hexavalent Chromium to avoid associated disadvantages, sees another process category for applying Conversion coatings especially for aluminum surfaces, a treatment with compositions based on the fluoroanions zircons and / or Titans (US-A-41 48 670, FR-A-942 789, EP-A-106 389, EP-A-825 280).
  • EP-B-700 452 envisages contacting surfaces of aluminum or its alloys with an aqueous solution prior to a second permanent anticorrosion treatment for pretreatment, comprising complex fluorides of the elements boron, Contain silicon, titanium, zirconium or hafnium individually or in admixture with each other in concentrations of the fluoro-anions of 100 to 4000 mg / l and have a pH of 0.3 to 3.5.
  • the parts made of aluminum or its alloys are subjected to a non-cutting and / or cutting deformation process, and / or bonded to one another or to parts made of steel and / or galvanized and / or alloy-galvanized steel by gluing and / or welding.
  • the application of the optionally polymers containing certain condition-containing solution can be done by spraying, dipping or no-rinse method, wherein in the case of the no-rinse method, the wet film amount between 2 to 10, preferably between 4 and 6 ml / m 2 metal surface should. Regardless of the form of application of the solution, it is advantageous to dry at temperatures between 40 and 85 ° C.
  • the parts made of aluminum or its alloys are acid or alkaline cleaned prior to the first conversion treatment, and cleaning steps and intermediate rinses with water and / or activating rinsing baths preferably take place before the permanent corrosion-protective treatment.
  • the object of the invention is to provide a method for Pre-treatment of workpieces with a surface made Aluminum or aluminum alloys for the non-cutting Forming and / or joining by welding or Gluing with similarly pretreated or optionally otherwise precoated workpieces or parts made of steel and / or galvanized and / or alloy galvanized Steel and a subsequent permanent anti-corrosive treatment by phosphating, by a chrome-free conversion treatment, by primer application or to provide painting regularly Workpieces with a sufficiently low Volume resistance with good adhesive pull shear values and good temporary Corrosion protection leads.
  • the compound of the invention pretreated workpieces can be pre-coated with similar pretreated or possibly otherwise, for.
  • phosphated workpieces done with surfaces of aluminum or its alloys. If intended to be joined to steel and / or galvanized and / or alloy galvanized steel parts, these parts may have bare or precoated surfaces.
  • a suitable pre-coating can, for. Example, a phosphate layer with a maximum coating weight of 2 g / m 2 or a layer of a conductive primer.
  • the pickling process is a Prevent cleaning / degreasing stage or the Pickling process is to lead in the way that one simultaneous cleaning / degreasing takes place. The latter can done by adding surfactant to the pickling solution.
  • a method for phosphating are those which with solutions based on zinc phosphate, in particular according to the low-zinc technology, or with Alkaline phosphate work, in the foreground.
  • the solutions can by adding further small amounts of polyvalent cations, such as calcium, magnesium, nickel, Copper or manganese, be modified.
  • chromium-free conversion treatment For chromium-free conversion treatment get in particular Acid solutions of the fluoro complexes of titanium, zirconium, Hafnium, but also boron and silicon, optionally with a content of organic polymer, used.
  • reaction primer As a primer so-called reaction primer or Adhesive base be applied.
  • the pretreatment of the workpieces according to the invention provides a sufficient, temporary corrosion protection for longer storage times safely. During this time takes place no negative influence on the weldability, in particular electrical resistance welding, or the bondability. Also is overlooking the Weldability ensures that the volume resistance Practical on all surface areas of the workpiece is equal to.
  • Workpieces in the context of the present invention are tape, Sheet metal and individual parts, such as profiles.
  • step c) The application of the solution according to step c) can be done by spraying or dipping with or without water rinsing. For application without water rinse, it is advantageous excess treatment solution by squeezing rollers too remove.
  • the treatment solution according to the roll coater method especially advantageous. It allows one in a single operation defined setting of the desired wet film thickness.
  • the workpiece is dried or the solution dried up.
  • Object temperatures of 30 to 90 ° C are special advantageous.
  • the treatment fluids are Usually concentrates used with low salt Water, preferably demineralized water, on each be diluted to be adjusted. Especially it is advantageous for the purpose of avoiding the entry of Alkali ions, the required fluoro anions of the zirconium and Titans with the help of the free acids and the If necessary, the respective pH value by adding ammonia adjust.
  • the pickling of the workpieces happens with a mineral acid-containing aqueous, acidic Solution. It can be carried out electrolytically or chemically. At the Electrolytic pickling is as mineral acid phosphoric acid particularly suitable. The pickling chemically, the because of the less complex apparatus in the Usually preference is given to using nitric acid or Nitric acid / hydrofluoric acid are made.
  • the surfactant, hydrogen fluoride and sulfuric acid contains, with solutions that are 3 to 8 g / l Sulfuric acid, 50 to 150 mg / l not complexed, free fluoride and 1 to 3 g / l nonionic surfactant ' contained, have been found to be particularly suitable.
  • Nonionic surfactants are ethylene oxide adducts Fatty alcohols and, for example, abietic acid especially suitable.
  • the measurement of the free fluoride was done with a fluoride-sensitive Electrode performed, with the calibration the electrode was made with solutions whose pH identical to that of the solution to be tested.
  • the pickling process should be carried out in such a way that a metal removal of about 0.1 to 0.6 g / m 2 workpiece surface is obtained.
  • step b) takes place preferably in several rinsing stages, being particularly advantageous, the rinse water cascade the workpiece to lead contrary. It should be the last Rinsing be carried out with demineralized water.
  • Treatment according to step c) prevents the ' Workpieces with a surface of aluminum or Aluminum alloy re-growth of an oxide layer occurs.
  • a further advantageous embodiment of the invention provides for the workpieces in step c) to be brought into contact with a solution containing colloidal silica. Due to the content of the solution of silica, the paint adhesion is improved in a subsequent coating. An adverse effect on the volume resistivity does not occur.
  • a particularly suitable silica is fumed silica having an average particle size of 10 to 25 nm.
  • Particularly advantageous coating weights are between 2 and 30 mg / m 2 (calculated as Si).
  • the silicic acid concentrations to be set in the respective treatment solutions used in stage c) can be determined in a simple manner on the basis of a few experiments. When applying the solution in the roll coater method, it can be easily calculated on the amount of wet film to be applied.
  • a lubricant acts in particular mineral oil-based forming oils containing fully synthetic or native, or um Dry lubricants based on polyethylene / polyacrylate.
  • the one perfect deformation and / or gluing or as a result of low and uniform over the workpiece surface Electric volume resistance is ongoing and allow easy welding.
  • the workpieces for a subsequent permanent Corrosion protection treatment ideally suited.
  • Example 2 shows that due to a too high Weight of the dressing in the treatment according to step c) obtained layer very high Volume resistances - especially after storage for 30 days - received become.
  • Examples 3 to 5 and 10 are indeed the obtained support weights in the desired range, however are due to the titanium / zirconium ratio in the Treatment solution for process step c) of about 1: 3 (Example 3) or about 3: 1 (Example 4) or as a result of Zirconium free (Example 5) or the freedom from titanium (Example 10) of the solution obtained Volume resistances, especially after 30 days Storage, unacceptable.

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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)
  • Application Of Or Painting With Fluid Materials (AREA)

Claims (5)

  1. Procédé de pré-traitement de pièces destinées à être soumises à un déformage sans enlèvement de copeaux ayant une surface en aluminium ou en alliage d'aluminium, et/ou à l'assemblage par soudure ou par collage avec des pièces usinées ayant subi un pré-traitement similaire, ou le cas échéant revêtues au préalable de manière différente, ou le cas échéant avec des pièces en acier et/ou en acier zingué et/ou en acier revêtu d'un alliage de zinc, le cas échéant préalablement revêtues, et ensuite à un traitement conférant une protection permanente contre la corrosion, par phosphatation, par un traitement de conversion exempt de chrome, par application d'une couche primaire ou par dépôt d'un vernis, dans lequel
    a) on décape les pièces avec des solutions acides aqueuses contenant des acides minéraux, par immersion ou pulvérisation,
    b) on rince avec de l'eau,
    c) on met en contact les pièces usinées avec une solution acide aqueuse, exempte de chrome et de polymère et qui est constituée essentiellement de Ti et Zr sous forme de fluorures complexes dans un rapport en poids de Ti/Zr allant de 2 :1 à 1 :2, ainsi que d'acide silicique colloïdal, de façon à ce que, après le séchage consécutif, il reste un poids de couche de 2 à 15mg/m2 ( calculé comme métal Ti/Zr), on utilise, lors de la mise en contact de la pièce usinée des solutions qui contiennent lors de l'application par immersion ou pulvérisation de 300 à 700 mg/l de fluorure (calculé comme anions fluorure) et qui présentent un pH allant de 4,0 à 5,0 et qui contiennent lors de l'application au rouleau de 5000 à 15000 mg/l de fluorure (calculé comme anions fluorure) et qui présentent un pH allant de 1,0 à 3,0.
  2. Procédé selon la revendication 1, dans lequel on décape les pièces à l'aide d'une solution contenant un tensioactif, de l'acide fluorhydrique et'de l'acide sulfurique.
  3. Procédé selon la revendication 2, dans lequel on décape les pièces à l'aide d'une solution qui contient de 3 à 8 g/l d'acide sulfurique, de 50 à 150 mg/l de fluorure libre et de 1 à 3 g/l de tensioactif non ionique.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel, dans le cas du pré-traitement de la pièce pour le déformage sans enlèvement de copeaux, on introduit un lubrifiant, avant l'opération de déformage.
  5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel on entreprend, préalablement au traitement conférant une protection permanente contre la corrosion, des traitements de nettoyage, de rinçage à l'eau et le cas échéant d'activation.
EP00925252A 1999-05-11 2000-04-29 Traitement prealable de surfaces d'aluminium a l'aide de solutions exemptes de chrome Expired - Lifetime EP1200641B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19921842 1999-05-11
DE19921842A DE19921842A1 (de) 1999-05-11 1999-05-11 Vorbehandlung von Aluminiumoberflächen durch chromfreie Lösungen
PCT/EP2000/003900 WO2000068458A1 (fr) 1999-05-11 2000-04-29 Traitement prealable de surfaces d'aluminium a l'aide de solutions exemptes de chrome

Publications (2)

Publication Number Publication Date
EP1200641A1 EP1200641A1 (fr) 2002-05-02
EP1200641B1 true EP1200641B1 (fr) 2003-12-17

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EP00925252A Expired - Lifetime EP1200641B1 (fr) 1999-05-11 2000-04-29 Traitement prealable de surfaces d'aluminium a l'aide de solutions exemptes de chrome

Country Status (10)

Country Link
US (1) US6562148B1 (fr)
EP (1) EP1200641B1 (fr)
AR (1) AR023943A1 (fr)
AT (1) ATE256765T1 (fr)
AU (1) AU4403400A (fr)
CA (1) CA2373089A1 (fr)
DE (2) DE19921842A1 (fr)
ES (1) ES2213012T3 (fr)
NO (1) NO20015445L (fr)
WO (1) WO2000068458A1 (fr)

Cited By (2)

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EP1870489B2 (fr) † 2006-04-19 2012-10-17 Ropal AG Méthode d'obtention d'un substrat brillant et anti-corrosion
US10125424B2 (en) 2012-08-29 2018-11-13 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates

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US7063735B2 (en) 2003-01-10 2006-06-20 Henkel Kommanditgesellschaft Auf Aktien Coating composition
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DE102005059314B4 (de) * 2005-12-09 2018-11-22 Henkel Ag & Co. Kgaa Saure, chromfreie wässrige Lösung, deren Konzentrat, und ein Verfahren zur Korrosionsschutzbehandlung von Metalloberflächen
US8673091B2 (en) * 2007-08-03 2014-03-18 Ppg Industries Ohio, Inc Pretreatment compositions and methods for coating a metal substrate
US9574093B2 (en) * 2007-09-28 2017-02-21 Ppg Industries Ohio, Inc. Methods for coating a metal substrate and related coated metal substrates
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PL2890829T3 (pl) 2012-08-29 2022-08-29 Ppg Industries Ohio, Inc. Kompozycje do obróbki wstępnej cyrkonu zawierające lit, związane z nimi sposoby obróbki substratów metalowych oraz powiązane z nimi powlekane substraty metalowe
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US9273399B2 (en) 2013-03-15 2016-03-01 Ppg Industries Ohio, Inc. Pretreatment compositions and methods for coating a battery electrode
HUE055428T2 (hu) * 2013-12-13 2021-11-29 Speira Gmbh Alumínium kompozit anyagok folyasztószer-mentes összekapcsolása
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DE102014225237B3 (de) * 2014-12-09 2016-04-28 Henkel Ag & Co. Kgaa Verfahren zur nasschemischen Vorbehandlung einer Vielzahl von Eisen- und Aluminiumbauteilen in Serie
CA2984597C (fr) 2015-05-01 2020-06-16 Novelis Inc. Procede de pretraitement de bobine continue
SI3303486T1 (sl) * 2015-06-03 2019-06-28 Atotech Deutschland Gmbh Sestavek za površinsko obdelavo
DE102015215651B4 (de) * 2015-08-17 2020-10-08 Vacuumschmelze Gmbh & Co. Kg Verfahren und Behandlungslösung zur Behandlung von Aluminiumbeschichtungen vor der Passivierung mit Chrom(III)-haltigen Lösungen
WO2017046139A1 (fr) * 2015-09-15 2017-03-23 Chemetall Gmbh Prétraitement de surfaces en aluminium avec des compositions contenant du zircon et du molybdène
JP6227749B2 (ja) * 2016-03-29 2017-11-08 株式会社神戸製鋼所 アルミニウム材の表面処理方法および表面処理アルミニウム材
KR20190043155A (ko) 2016-08-24 2019-04-25 피피지 인더스트리즈 오하이오 인코포레이티드 금속 기판을 처리하기 위한 알칼리성 조성물
EP3456864B1 (fr) 2017-09-18 2019-11-13 Henkel AG & Co. KGaA Prétraitement d'aluminium, en particulier d'alliages d'aluminium, à deux étapes comprenant le bain de décapage et le traitement de conversion
WO2020148412A1 (fr) 2019-01-18 2020-07-23 Constellium Neuf-Brisach Traitement continu de surface de bobines constituées de feuilles d'alliages d'aluminium
FR3091880B1 (fr) * 2019-01-18 2022-08-12 Constellium Neuf Brisach Traitement de surface en continu des bobines réalisées à partir de tôles d’alliages d’aluminium
JP6846558B1 (ja) * 2019-09-27 2021-03-24 株式会社Uacj アルミニウム合金材及びその製造方法

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Publication number Priority date Publication date Assignee Title
EP1870489B2 (fr) † 2006-04-19 2012-10-17 Ropal AG Méthode d'obtention d'un substrat brillant et anti-corrosion
US8993119B2 (en) 2006-04-19 2015-03-31 Ropal Europe Ag Process for producing a corrosion-protected and high-gloss substrate
US10125424B2 (en) 2012-08-29 2018-11-13 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates
US10920324B2 (en) 2012-08-29 2021-02-16 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing molybdenum, associated methods for treating metal substrates, and related coated metal substrates

Also Published As

Publication number Publication date
WO2000068458A1 (fr) 2000-11-16
AR023943A1 (es) 2002-09-04
US6562148B1 (en) 2003-05-13
ES2213012T3 (es) 2004-08-16
EP1200641A1 (fr) 2002-05-02
CA2373089A1 (fr) 2000-11-16
DE19921842A1 (de) 2000-11-16
NO20015445D0 (no) 2001-11-07
AU4403400A (en) 2000-11-21
ATE256765T1 (de) 2004-01-15
DE50004805D1 (de) 2004-01-29
NO20015445L (no) 2001-11-07

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