EP4249634A1 - Procédé de modification d'une surface d'une tôle d'acier revêtue par immersion à chaud - Google Patents

Procédé de modification d'une surface d'une tôle d'acier revêtue par immersion à chaud Download PDF

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Publication number
EP4249634A1
EP4249634A1 EP23161660.8A EP23161660A EP4249634A1 EP 4249634 A1 EP4249634 A1 EP 4249634A1 EP 23161660 A EP23161660 A EP 23161660A EP 4249634 A1 EP4249634 A1 EP 4249634A1
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EP
European Patent Office
Prior art keywords
coating
aqueous solution
inorganic acid
steel sheet
bis
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.)
Withdrawn
Application number
EP23161660.8A
Other languages
German (de)
English (en)
Inventor
Burak William Cetinkaya
Fabian JUNGE
Tobias LEWE
Eugen Sabunow
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.)
ThyssenKrupp Steel Europe AG
Original Assignee
ThyssenKrupp Steel Europe AG
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 ThyssenKrupp Steel Europe AG filed Critical ThyssenKrupp Steel Europe AG
Publication of EP4249634A1 publication Critical patent/EP4249634A1/fr
Withdrawn legal-status Critical Current

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    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/53—Treatment of zinc 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
    • C23C22/06—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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron 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
    • 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
    • C23G1/10—Other heavy metals

Definitions

  • the invention relates to a method for modifying a surface of a hot-dip coated Zn-Al-Mg coating on a steel sheet.
  • hot-dip coated steel sheets have different influences on the chemical composition of the immediate surface of the zinc-based coating.
  • the aging of a particularly alloyed surface in air or other atmospheres can influence and change the composition of areas near the surface.
  • Changing the surface chemistry of the zinc-based coating can have an impact on further processing steps such as pretreatment, bonding, phosphating and/or painting.
  • the superficial oxide layer on the Zn-Al-Mg coating up to a depth of up to approx. 100 nm can lead to a negative property profile, but also the components of the coating underneath, especially after aging, can be a hindrance to subsequent processes and for the achievement of the corresponding process and surface-relevant properties.
  • binary (zinc-magnesium) or ternary (zinc-aluminum-magnesium) eutectic phases occur locally to varying degrees between, above and below the primarily precipitated zinc grains.
  • These eutectic phases are made up of the eutectic and pure metals, i.e. H.
  • these eutectic phases also have (secondary) zinc grains and possibly Al grains.
  • These secondary zinc grains and possibly Al grains should not be confused with the primarily precipitated zinc grains (primary zinc grains), since they have a volume that is several orders of magnitude smaller than the primary zinc grains.
  • the primary zinc grains sometimes have a diameter of over 30 ⁇ m
  • the diameter of the secondary zinc grains in the eutectic phases is up to 2 ⁇ m. Furthermore, these secondary grains are precipitated before or after the eutectic.
  • the eutectic phases described above are referred to as hypo- or hyper-eutectic phases, depending on whether they are precipitated before or after the eutectic.
  • the layer structure of a Zn-Al-Mg coating has a non-extensive, distributed enrichment of eutectic phases that are arranged above the zinc grains (and possibly also in the zinc grains).
  • the eutectic and the eutectic phases are magnesium-rich phases, for example in comparison to the primary tin grains.
  • the aging of the Zn-Al-Mg coatings when stored in air or in oxygen-containing atmospheres can result in a change in the chemical composition of the layers near the surface, and thus also lead to the formation and growth of oxides and oxide layers in and on the metallic coating.
  • the formation and growth of these oxides and oxide layers is associated with the penetration of oxygen into the eutectic phases of the protective layer and leads to additional deterioration in further processing.
  • elementary metal atoms from the eutectic and the eutectic phases are oxidized to form oxides and/or hydroxides or similar compounds (metal oxides).
  • phase rich in zinc and/or aluminum are hardly oxidized.
  • the metal oxides are arranged in layers close to the surface, i.e. in the upper layers of the coating, in particular at a depth of up to 75 nm.
  • the object of the present invention is to provide a method for modifying a surface of a hot-dip coated steel sheet, with which magnesium-rich phases from the layer of the coating near the surface and/or the magnesium-rich native oxide layer on the coating can be at least partially removed, in particular without losses in terms of on the production speed.
  • the invention relates to a method for modifying a surface of a hot-dip coated Zn-Al-Mg coating on a steel sheet, the coating being wetted with an aqueous solution of an inorganic acid, an aqueous solution of an inorganic acid having a pH value less than 0, 01, especially less than 0, is used.
  • the modification of the surface of the coating is to be designed three-dimensionally in the sense of the present invention. Either defined areas of the surface or the surface are completely wetted with an aqueous solution of an inorganic acid.
  • An aqueous solution of an inorganic acid with a pH value of less than 0.01, in particular less than 0, is used, so that although two-dimensional areas are wetted, the wetting acts in layers of the coating close to the surface, i.e. in the depth and thus in the third Dimension.
  • the surface of the hot-dip coated Zn-Al-Mg coating on the steel sheet can be modified by an aqueous solution of an inorganic acid with a pH value of less than 0.01, in particular less than 0, in such a way that disruptive elements are removed the coating and/or in the layer of the coating near the surface can be removed, so that further processing steps, such as gluing, can be carried out effectively.
  • the pH value is a measure of the concentration or activity of hydrogen ions (H + ) or hydronium ions (also called oxonium, hydrooxonium; H 3 O + ) in a solution.
  • the numerical value indicates the concentration as a negative decadal logarithm. The fewer hydrogen ions there are in a solution, the greater the pH.
  • Acidic solutions have a pH of less than 7.0. The pH value of solutions can be calculated from the original concentration of an acid using various approximate equations.
  • any acid which produces a concentration of hydrogen ions with a molarity of more than 1 has a negative pH value.
  • strong acids do not completely dissociate at high concentrations, the influence of hydrogen ions in the solution is enhanced because there is so little water per acid formula unit.
  • the activity of the hydrogen ions is much higher than the actual concentration. Therefore, the pH value calculated as described above in the sense of the invention is the pH value of the aqueous solution to be used according to the invention.
  • the coating comprises a zinc alloy with, in addition to zinc (rest) and unavoidable impurities, additional elements such as aluminum with a content between 0.1 and 10.0% by weight and magnesium with a content between 0.1 and 10.0% by weight .-%.
  • additional elements such as aluminum with a content between 0.1 and 10.0% by weight and magnesium with a content between 0.1 and 10.0% by weight .-%.
  • impurities elements from the group Si, Sb, Pb, Ti, Ca, Mn, Sn, La, Ce and Cr can be contained in the coating individually or in combination with a total of up to 0.5% by weight.
  • Steel sheets or steel sheet components made from them with a zinc-based corrosion protection coating have very good cathodic corrosion protection, which have been used in automobile construction for years.
  • the coating has magnesium with a content of at least 1.0% by weight, in particular at least 1.1% by weight, preferably at least 1.3% by weight and aluminum with a content of at least 1. 0% by weight, in particular at least 1.1% by weight.
  • the thickness of the coating can be between 1.5 and 15 ⁇ m, in particular between 2 and 12 ⁇ m, preferably between 3 and 10 ⁇ m.
  • an inorganic acid is selected from the group containing or consisting of: H 2 SO 4 , HCl, HNO 3 , H3PO 4 , H 2 SO 3 , HNO 2 , H 3 PO 3 , HF, or a mixture of 2 or several of these acids are used as an aqueous solution.
  • so-called super acids such as fluorosulfonic acid (HSO 3 F) or fluoroantimonic acid (HSbF 6 ) are used or mixed with the aforementioned inorganic acids.
  • the pH value is not less than -10, in particular not less than -8, preferably not less than -6, preferably not less than -4.
  • the coating is wetted with the aqueous solution of an inorganic acid for a time of 0.1 to 2 s and at a temperature of 10 ° C to 90 ° C.
  • the coating is applied for a time of at least 0.1 s, in particular at least 0.2 s, preferably at least 0.3 s, 0.4 s, preferably at least 0.5 s, and a maximum of 2 s, in particular a maximum of 1.8 s , preferably a maximum of 1.5 s, 1.4 s, 1.3 s, preferably a maximum of 1.2 s, 1.1 s, 1.0 s, wetted with an aqueous solution of an inorganic acid.
  • the coating is wetted with an aqueous solution of an inorganic acid at a temperature of 10 °C to 90 °C, in particular 20 °C to 70 °C, preferably 20 °C to 50 °C, preferably 20 °C to 40 °C , particularly preferably 20 °C to 30 °C.
  • the coating is wetted by spraying, spraying, dipping or applying an aqueous solution of an inorganic acid.
  • an aqueous solution of an inorganic acid is applied to the coating using a process selected from the group or consisting of spraying, spraying, dipping or application (coil coating process).
  • the coating is preferably wetted continuously with an aqueous solution of an inorganic acid.
  • the wetting is ended by rinsing with water and/or an aqueous solution.
  • the wetting with an aqueous solution of an inorganic acid is interrupted by rinsing with water and/or an alcohol, for example selected from the group containing or consisting of methanol, ethanol, propanol, isopropanol, ethanol, in particular isopropanol, or an aqueous solution.
  • rinsing takes place in 2 steps, in a first step with water; in a second sub-step with an alcohol or an aqueous solution of an alcohol as stated above.
  • rinsing is carried out with water and an alcohol in one step, preferably as a mixture of water with one of the alcohols specified above.
  • the rinsing is preferably carried out continuously, in particular one method selected from the group or consisting of spraying, spraying, dipping and application (coil coating process).
  • drying is preferably carried out by rinsing, with the “rinsed” coating preferably being dried by increasing the temperature (up to a maximum of 100 ° C) or by using a fan.
  • the “rinsed” coating is air-dried, for example without any additional aids.
  • a polymer which is an adhesive and/or varnish, is applied to the modified surface of the coating on a steel sheet, as described above.
  • a further substrate is selected from the group containing or consisting of: substrate treated according to the invention, i.e. steel sheet, steel sheet not treated according to the invention, metal sheet, plastic.
  • the present invention also relates to the use of an aqueous solution of an inorganic acid with a pH of less than 0.01, as described above, for the surface removal of a hot-dip coated Zn-Al-Mg coating on a steel sheet, as described above, up to a Depth of at least 100 nm, in particular at least 120 nm, 125 nm, 150 nm, 175 nm, 200 nm, 250 nm, 300 nm, preferably at least 400 nm, preferably at least 500 nm up to a maximum of 2 ⁇ m, for example within a time of 0 ,1 to 2 s, at least 0.1 s, in particular at least 0.2 s, preferably at least 0.3 s, 0.4 s, preferably at least 0.5 s, and a maximum of 2 s, in particular a maximum of 1.8 s, preferably a maximum of 1.5 s, 1.4 s, 1.3 s, preferably a maximum of 1.2
  • an aqueous solution for example Ridoline C72
  • an aqueous solution for example Bonderite C-IC 124 N
  • wetting was carried out by application (using the coil coating process) and the time in both cases was approx. 1 s and 25 °C. In both cases, the wetting was ended by rinsing with water and the rinsed steel strips were then dried using a short-term temperature increase to approx. 80 ° C.
  • Several steel sheet samples were separated from the first steel strip, R as reference, and from the second steel strip, E as invention, in order to enable a representative and comparable result.
  • a surface of a hot-dip coated Zn-Al-Mg coating on a steel sheet can be modified in such a way that disruptive elements on the coating and/or in the layer of the coating near the surface can be removed, so that further processing steps, for example gluing, which can lead to an improved fracture pattern, can be carried out effectively, which could be demonstrated using the exemplary embodiment and comparison with a reference.

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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)
EP23161660.8A 2022-03-22 2023-03-14 Procédé de modification d'une surface d'une tôle d'acier revêtue par immersion à chaud Withdrawn EP4249634A1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102022106615.0A DE102022106615A1 (de) 2022-03-22 2022-03-22 Verfahren zum Modifizieren einer Oberfläche eines schmelztauchbeschichteten Stahlblechs

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EP4249634A1 true EP4249634A1 (fr) 2023-09-27

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EP23161660.8A Withdrawn EP4249634A1 (fr) 2022-03-22 2023-03-14 Procédé de modification d'une surface d'une tôle d'acier revêtue par immersion à chaud

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EP (1) EP4249634A1 (fr)
DE (1) DE102022106615A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2474649A1 (fr) * 2011-01-05 2012-07-11 Voestalpine Stahl GmbH Procédé de traitement de surface d'un substrat ayant un revêtement de protection
JP2017145503A (ja) * 2016-02-18 2017-08-24 Ｊｆｅスチール株式会社 皮膜付溶融Ｚｎ−Ａｌ−Ｍｇ系めっき鋼板およびその製造方法
DE102018216317A1 (de) 2018-09-25 2020-03-26 Thyssenkrupp Ag Verfahren zur Modifikation von feuerverzinkten Oberflächen
DE102019204224A1 (de) 2019-03-27 2020-10-01 Thyssenkrupp Steel Europe Ag Verfahren zur Neukonditionierung von feuerverzinkten Oberflächen
DE102019134298A1 (de) 2019-12-13 2021-06-17 Thyssenkrupp Steel Europe Ag Verfahren zum Herstellen eines Stahlflachprodukts mit einer metallischen Schutzschicht auf Basis von Zink und einer auf einer Oberfläche der metallischen Schutzschicht erzeugten Phosphatierschicht und derartiges Stahlflachprodukt

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2474649A1 (fr) * 2011-01-05 2012-07-11 Voestalpine Stahl GmbH Procédé de traitement de surface d'un substrat ayant un revêtement de protection
JP2017145503A (ja) * 2016-02-18 2017-08-24 Ｊｆｅスチール株式会社 皮膜付溶融Ｚｎ−Ａｌ−Ｍｇ系めっき鋼板およびその製造方法
DE102018216317A1 (de) 2018-09-25 2020-03-26 Thyssenkrupp Ag Verfahren zur Modifikation von feuerverzinkten Oberflächen
DE102019204224A1 (de) 2019-03-27 2020-10-01 Thyssenkrupp Steel Europe Ag Verfahren zur Neukonditionierung von feuerverzinkten Oberflächen
DE102019134298A1 (de) 2019-12-13 2021-06-17 Thyssenkrupp Steel Europe Ag Verfahren zum Herstellen eines Stahlflachprodukts mit einer metallischen Schutzschicht auf Basis von Zink und einer auf einer Oberfläche der metallischen Schutzschicht erzeugten Phosphatierschicht und derartiges Stahlflachprodukt

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