EP1200641A1 - 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

Info

Publication number
EP1200641A1
EP1200641A1 EP00925252A EP00925252A EP1200641A1 EP 1200641 A1 EP1200641 A1 EP 1200641A1 EP 00925252 A EP00925252 A EP 00925252A EP 00925252 A EP00925252 A EP 00925252A EP 1200641 A1 EP1200641 A1 EP 1200641A1
Authority
EP
European Patent Office
Prior art keywords
workpieces
treatment
aluminum
free
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.)
Granted
Application number
EP00925252A
Other languages
German (de)
English (en)
Other versions
EP1200641B1 (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
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 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

Links

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 pretreating workpieces with a surface made of aluminum or aluminum alloys for non-cutting shaping and / or joining by welding or gluing with similarly pretreated or possibly otherwise pre-coated workpieces or with pretreated parts made of steel and / or galvanized and / or or galvanized steel as well as for a subsequent corrosion protection treatment Phosphating, through a chrome-free conversion treatment, by primer application or by painting.
  • connection of the parts is followed by a corrosion protection treatment, depending on the
  • the properties of the connected parts can consist of a phosphating treatment, a chrome-free conversion treatment, a primer application or a paint job.
  • EP-B-700 452 provides for surfaces of aluminum or its alloys to be brought into contact with an aqueous solution which contains complex fluorides of the elements boron, prior to a second permanent corrosion-protective treatment for pretreatment. Contain silicon, titanium, zirconium or hafnium individually or in a mixture with one another in concentrations of the fluoro anions of a total of 100 to 4000 mg / 1 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 process, and / or connected to one another or to parts made of steel and / or galvanized and / or alloy-galvanized steel by gluing and / or welding.
  • the solution which may contain polymers of a certain nature, can be applied by spraying, dipping or the no-rinse process, in the case of the no-rinse process the amount of wet film being between 2 and 10, preferably between 4 and 6, ml / m 2 of 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 before the first conversion treatment, preferably cleaning steps and intermediate rinsing with water and / or with activating rinsing baths are carried out before the permanent corrosion-protecting treatment.
  • the object of the invention is to provide a method for pretreating workpieces with a surface made of aluminum or aluminum alloys for non-cutting shaping and / or joining by welding or gluing with workpieces pretreated in the same way or, if necessary, otherwise coated, or with parts made of steel and / or galvanized and / or galvanized alloy steel and a subsequent permanent corrosion protection treatment by phosphating, by a chromium-free conversion treatment, by primer application or painting, which regularly leads to workpieces with a sufficiently low volume resistance with good adhesive tensile shear values and good temporary corrosion protection values.
  • the method of the type mentioned according to the invention is designed in such a way that the workpieces a) pickling with an aqueous acidic solution containing mineral acid by immersion or spraying, b) rinsing with water, c) using an aqueous, acidic solution which is free of chromium and polymers and contains Ti and Zr as complex fluorides in a weight ratio of Ti: Contains Zr from 2: 1 to 1: 2, in such a way that after the subsequent drying results in a layer weight of 2 to 15 mg / m 2 (calculated as Ti / Zr metal),
  • solutions when bringing the workpiece into contact, solutions are used which contain 300 to 700 mg / 1 fluoride (calc. as fluoro-anion) when dipped or sprayed and have a pH of 4.0 to 5.0 and when applied in a roll application process contain 5000 to 15000 mg / 1 fluoride (calculated as fluoro-anion) and have a pH of 1.0 to 3.0.
  • the workpieces are pickled with an aqueous acidic solution containing mineral acid by dipping or spraying.
  • An alkaline cleaning for example, has the formation of titanium / zircon layers with poor
  • volume resistance values result. The same applies to layers which are obtained using polymer-containing solutions, which is why the solutions to be used within the process according to the invention must be polymer-free.
  • the cleaning process must be preceded by a cleaning / degreasing step or Pickling process must be carried out in such a way that simultaneous cleaning / degreasing takes place. The latter can be done by adding surfactant to the pickling solution.
  • reaction primers or primers can be applied as primers.
  • the pretreatment of the workpieces according to the invention ensures adequate, temporary corrosion protection for longer storage times. During this time there is no negative influence on the weldability, in particular the electrical resistance welding, or the bondability. With regard to the weldability, it is also ensured that the volume resistance is practically the same on all surface areas of the workpiece.
  • Workpieces in the sense of the present invention are strip, sheet metal and individual parts, such as profiles.
  • the solution according to stage c) can be applied in spraying or immersion with or without water rinsing. When applied without water rinsing, it is advantageous to remove excess treatment solution by squeezing rollers.
  • the application of the treatment solution using the roll coater process is particularly advantageous. It allows a defined setting of the desired wet film thickness in one operation.
  • the workpiece is dried or the solution is dried.
  • Object temperatures from 30 to 90 ° C are particularly advantageous.
  • concentrates are usually used, which are diluted with low-salt water, preferably fully demineralized water, to the concentrations to be set in each case.
  • low-salt water preferably fully demineralized water
  • the workpieces (process stage a)) are pickled with an aqueous acidic solution containing mineral acid. It can be carried out electrolytically or chemically.- In the case of electrolytic pickling, phosphoric acid is particularly suitable as the mineral acid.
  • Chemical pickling which is generally preferred due to the less complex work involved in apparatus, can be carried out using nitric acid or nitric acid / hydrofluoric acid.
  • the workpieces are pickled with a solution in spraying or dipping which contains surfactant, hydrogen fluoride and sulfuric acid, solutions containing 3 to 8 g / 1 sulfuric acid, 50 to 150 mg / 1 not complex-bound, free Fluoride and 1 to 3 g / 1 non-ionic surfactant have been found to be particularly suitable.
  • Ethylene oxide adducts with fatty alcohols and, for example, abietic acid are particularly suitable as nonionic surfactants.
  • the measurement of the free fluoride was carried out with a fluoride-sensitive electrode, the calibration of the electrode being carried out with solutions whose pH was 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 approximately 0.1 to 0.6 g / m 2 of the workpiece surface is obtained.
  • the water rinsing subsequent to the pickling of the workpieces - in accordance with stage b) - is preferably carried out in several rinsing stages, it being particularly advantageous to guide the rinsing water in the manner of a cascade against the workpiece.
  • the last rinse step should be carried out with deionized water.
  • the treatment according to stage c) following the pickling and rinsing stage prevents an oxide layer from growing again on the workpieces with a surface made of aluminum or aluminum alloy.
  • 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.
  • the silicic acid content of the solution improves the paint adhesion in a subsequent painting.
  • the volume resistance is not adversely affected.
  • a particularly suitable silica is pyrogenic silica with 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 silica concentrations to be set in the respective treatment solutions used in stage c) can be determined in a simple manner using a few experiments. When the solution is applied using the roll coater process, it can easily be calculated from the amount of wet film to be applied.
  • a further advantageous embodiment of the invention provides for a lubricant to be applied to the workpieces.
  • a lubricant to be applied to the workpieces.
  • These are, in particular, mineral oil-based forming oils, which can be fully synthetic or native, or dry lubricants based on polyethylene / polyacrylate.
  • Activation treatment for example with an activating agent containing titanium and phosphate.
  • workpieces with layers are regularly obtained which permit perfect deformation and / or gluing or, owing to the low electrical volume resistance which is uniform over the workpiece surface, allow flawless and problem-free welding. Beyond that the workpieces are ideally suited for a subsequent, permanently corrosion-protective treatment.
  • nonionic surfactant consisting of ethoxylated fatty alcohol and ethoxylated abietic acid in a weight ratio of 1: 1.
  • the pickling process was carried out in such a way that the
  • the workpieces were then rinsed thoroughly with water, in the last stage with demineralized water.
  • the measured on the single sheet Volume resistances were 6 to 8 ⁇ -ohms for alloy AA 5182 and 9 to 11 ⁇ -ohms for alloy AA 6016.
  • the solutions which were at room temperature were applied by immersion or according to the roll coater method, the immersion duration or wet film thickness being selected in such a way that that in column 2 of Table 2 mentioned weights (calculated as titanium or zirconium metal) resulted.
  • excess treatment solution was removed by squeezing and then the treated surface was dried.
  • the drying or drying on the roll coater application was carried out at 60 ° C in each case.
  • the adhesive tensile shear values were determined using tensile shear tests in accordance with DIN 53283 using a commercially available two-component epoxy adhesive.
  • the first row of column 4 of Table 2 gives the measured values which were obtained immediately after the bonding, the second row shows the measured values which were obtained after 30 days of salt spray-condensation alternating test in accordance with VDA 621-415.
  • Example 2 shows that very high volume resistances - especially after storage for 30 days - are obtained as a result of the coating weight being too high for the layer obtained in the treatment according to stage c).
  • the coating weights obtained are in the desired range, but are due to the titanium / zirconium ratio in the treatment solution for process stage c) of approximately 1: 3
  • Example 3 or approx. 3: 1 (Example 4) or due to the absence of zirconium (Example 5) or the absence of titanium
  • Examples 6 to 9 and 11 to 13 show that if the conditions essential to the invention are observed with regard to the type of pickling treatment, the Ti / Zr ratio, the coating weight produced, the respective concentration and pH ranges of the treatment solutions, layers with extremely good volume resistances are added good adhesive properties are obtained at the same time.

Abstract

L'invention concerne un procédé pour le traitement préalable de pièces présentant une surface en aluminium ou en alliage d'aluminium, destinées à subir un formage et/ou un assemblage par soudure ou collage avec des pièces traitées préalablement de la même façon ou, éventuellement, prérecouverte d'une autre façon, ou bien avec des pièces, éventuellement prérecouvertes, en acier et/ou en acier zingué et/ou en acier recouvert d'alliage. Selon ledit procédé, lesdites pièces sont également soumises à un traitement consécutif destiné à les protéger en permanence contre la corrosion. Le procédé présenté comprend trois étapes: (a) rinçage des pièces avec une solution acide aqueuse contenant un acide minéral; (b) rinçage des pièces avec de l'eau; (c) mise en contact des pièces avec une solution aqueuse, acide, exempte de chrome et de polymères, qui contient du Ti et du Zr comme fluorures complexes, selon un rapport pondéral Ti:Zr = 2:1-1:2, de telle sorte qu'après le séchage subséquent le grammage de la couche soit de 2 à 15 mg/m2 (calculé en tant que Ti ou Zr), cette opération étant réalisée, en fonction de la forme d'application, avec des solutions présentant des concentrations et des valeurs de pH différentes.
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
DE19921842A DE19921842A1 (de) 1999-05-11 1999-05-11 Vorbehandlung von Aluminiumoberflächen durch chromfreie Lösungen
DE19921842 1999-05-11
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 true EP1200641A1 (fr) 2002-05-02
EP1200641B1 EP1200641B1 (fr) 2003-12-17

Family

ID=7907793

Family Applications (1)

Application Number Title Priority Date Filing Date
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) NO20015445D0 (fr)
WO (1) WO2000068458A1 (fr)

Cited By (2)

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WO2017046139A1 (fr) * 2015-09-15 2017-03-23 Chemetall Gmbh Prétraitement de surfaces en aluminium avec des compositions contenant du zircon et du molybdène
US10400337B2 (en) 2012-08-29 2019-09-03 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing lithium, associated methods for treating metal substrates, and related coated metal substrates

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US6488990B1 (en) * 2000-10-06 2002-12-03 Chemetall Gmbh Process for providing coatings on a metallic surface
JP2004521187A (ja) 2001-02-16 2004-07-15 ヘンケル・コマンディットゲゼルシャフト・アウフ・アクチエン 多金属物品を処理する方法
US7063735B2 (en) 2003-01-10 2006-06-20 Henkel Kommanditgesellschaft Auf Aktien Coating composition
MXPA05006053A (es) 2003-01-10 2005-08-16 Henkel Kgaa Una composicion de revestimiento.
DE10358590A1 (de) * 2003-12-12 2005-07-07 Newfrey Llc, Newark Verfahren zur Vorbehandlung von Oberflächen von Schweissteilen aus Aluminium oder seinen Legierungen und entsprechende Schweissteile
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
EP1870489B2 (fr) * 2006-04-19 2012-10-17 Ropal AG Méthode d'obtention d'un substrat brillant et anti-corrosion
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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US8282801B2 (en) * 2008-12-18 2012-10-09 Ppg Industries Ohio, Inc. Methods for passivating a metal substrate and related coated metal substrates
HUE039960T2 (hu) 2012-08-29 2019-02-28 Ppg Ind Ohio Inc Molibdéntartalmú cirkóniumos elõkezelõ összetételek, fémes hordozók kezelésére szolgáló kapcsolódó eljárások, valamint bevonatolt fémes hordozók
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EP3303486B1 (fr) 2015-06-03 2019-03-20 ATOTECH Deutschland GmbH Composition de traitement de surface
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
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
US11518960B2 (en) 2016-08-24 2022-12-06 Ppg Industries Ohio, Inc. Alkaline molybdenum cation and phosphonate-containing cleaning composition
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
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US10400337B2 (en) 2012-08-29 2019-09-03 Ppg Industries Ohio, Inc. Zirconium pretreatment compositions containing lithium, associated methods for treating metal substrates, and related coated metal substrates
WO2017046139A1 (fr) * 2015-09-15 2017-03-23 Chemetall Gmbh Prétraitement de surfaces en aluminium avec des compositions contenant du zircon et du molybdène
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Also Published As

Publication number Publication date
ES2213012T3 (es) 2004-08-16
WO2000068458A1 (fr) 2000-11-16
DE19921842A1 (de) 2000-11-16
ATE256765T1 (de) 2004-01-15
CA2373089A1 (fr) 2000-11-16
US6562148B1 (en) 2003-05-13
NO20015445L (no) 2001-11-07
EP1200641B1 (fr) 2003-12-17
AU4403400A (en) 2000-11-21
DE50004805D1 (de) 2004-01-29
AR023943A1 (es) 2002-09-04
NO20015445D0 (no) 2001-11-07

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