EP3103897A1 - Procédé de séparation électrochimique de couches anorganiques minces - Google Patents

Procédé de séparation électrochimique de couches anorganiques minces Download PDF

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Publication number
EP3103897A1
EP3103897A1 EP15171740.2A EP15171740A EP3103897A1 EP 3103897 A1 EP3103897 A1 EP 3103897A1 EP 15171740 A EP15171740 A EP 15171740A EP 3103897 A1 EP3103897 A1 EP 3103897A1
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EP
European Patent Office
Prior art keywords
substrate
electrolyte
coating
metallic
potential
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Withdrawn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
EP15171740.2A
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German (de)
English (en)
Inventor
Matthias Kimpel
Stefan Krebs
Thomas Lostak
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
ThyssenKrupp AG
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ThyssenKrupp Steel Europe AG
ThyssenKrupp AG
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Application filed by ThyssenKrupp Steel Europe AG, ThyssenKrupp AG filed Critical ThyssenKrupp Steel Europe AG
Priority to EP15171740.2A priority Critical patent/EP3103897A1/fr
Publication of EP3103897A1 publication Critical patent/EP3103897A1/fr
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
    • C25D9/10—Electrolytic coating other than with metals with inorganic materials by cathodic processes on iron or steel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation

Definitions

  • the invention relates to a method for the electrochemically assisted deposition of particularly thin inorganic layers on a metallic, electrically conductive substrate, which is held in an electrolyte during the deposition process.
  • the invention relates to a method for accelerated deposition of so-called “conversion layers” on flat steel products.
  • conversion layers flat steel products
  • flat steel products from rolled steel sheets or strips as well as blanks, blanks and the like obtained from it are called.
  • Flat steel products, but also other corrosion-susceptible metallic substrates, are usually provided with a multilayer coating system to improve their corrosion resistance and to optimize their optical appearance.
  • the respective substrate is first provided with a metallic protective layer, in particular an alloy layer based on zinc, magnesium or aluminum.
  • This metallic protective layer sacrifices itself in a corrosive attack and protects in this way the underlying corrosion-sensitive metal.
  • the conversion layer which is typically an inorganic phosphate layer, is usually wet-chemically applied to the metallic protective layer or, if omitted, directly onto the uncoated metal substrate. On the one hand, this conversion layer protects the metallic protective layer or the metal substrate against corrosive attacks.
  • the conversion layer improves the bonding of a subsequently applied organic coating to the protective layer or the metallic substrate.
  • the outer organic coating which is typically a paint or a laminated polymer layer, also serves as protection against contact with water and associated oxidation, and additionally has a decorative function.
  • the lifetime of coating composite systems of the type described above is determined in principle by the interfacial chemistry of the different phase boundaries between the individual layers.
  • the composite "metallic substrate / metallic protective layer” is here, as far as its durability considered, usually considered as uncritical due to the chemical relationship of the interconnected substances.
  • the phase boundary between the metallic substrate or the metallic protective layer applied thereto and the outer organic coating proves to be significantly more complex.
  • a fundamental problem here is that the outer coating is usually semipermeable for corrosive media, especially oxygen and water. As a result, at least locally, an electron transfer reaction may occur at the interface between the metal of the substrate or the metallic protective layer and the polymer of the outer coating. The result is a corrosion process in which the metallic substrate or the metallic protective layer optionally present thereon is anodically oxidized. At the same time, oxygen is cathodically reduced to hydroxyl ions, which can lead to a substrate-near alkalization of the composite interface and to a delamination of the outer coating.
  • a conversion layer is built up on the metal substrate to be protected or the metallic protective layer applied thereon, on which then lies the outer polymer layer.
  • Zr-based conversion layers in which an acidic pickling attack of the metal surface to be treated achieves a local alkalization of the interface, so that a thin ZrO.sub.2 layer precipitates.
  • the principal mechanisms for the deposition of these Zrbasierenden conversion layers are described in the literature ( P. Puomi, HM Fagerholm, JB Rosenholm, K. Jyrhims, Comparison of different commercial pretreatment methods for hot-dip galvanized and galfan coated steel, Surface and Coatings Technology 115 (1999) 70-78 ; P. Puomi, HM Fagerholm, JB Rosenholm, R.
  • the layer deposition could be significantly accelerated by means of Cu 2+ ions ( T. Lostak, S. Krebs, A. Maljusch, T. Gothe, M. Giza, M. Kimpel, J. Flock, S. Schulz, Formation and characterization of Fe3 + / Cu2 + -modified zirconium oxide conversion layers on zinc alloy coated steel sheets, Electrochimica Acta 112 (2013) 14-23 ).
  • Fast-moving coating processes require pretreatment systems whose deposition kinetics are sufficiently high to produce a closed conversion layer at short contact times with the conversion bath.
  • the film formation kinetics can be significantly increased. Often these additives are toxic or ecologically questionable for other reasons. Therefore, alternative processes are sought, with which layers can be accelerated on the respective substrate.
  • the aim of this procedure is a method which makes it possible to build the thin film serving as adhesion promoter between the respective substrate and a lacquer layer applied in a following process step on the substrate so fast that the method can be included in a continuous overall process the substrate is suitably provided and subsequently painted.
  • the provision of the substrate may include a metallic corrosive attack protective layer coating included in the continuous process of the overall process.
  • the flat product is cleaned with an alkaline detergent, then rinsed with demineralized water and then dried.
  • a conversion solution is applied which contains in aqueous solution a Zr or Ti compound which dissociates into zirconium or titanium fluoro complexes.
  • a conversion layer is generated, according to a first Alternatively, the conversion solution as an adhesion promoter additionally an organosilane is added, which contains an epoxy group and is water-soluble, whereas according to a second alternative, first the conversion solution is applied to the flat product, then the flat product rinsed with demineralized water or service water and then an aqueous solution of a suitable adhesion promoter serving organosilane containing an epoxy group is applied. Finally, the resulting flat product is dried.
  • the invention has achieved this object by a method with the steps specified in claim 1.
  • the invention proposes the surface of the substrate to be coated with the inorganic coating is cathodically polarized during the residence in the electrolyte.
  • the invention is based on the idea of polarizing the substrate to be coated, which is moved in an electrolyte, such that the desired thin inorganic conversion layer forms on the electrically conductive substrate surface. According to the invention, the application of the thin coating is therefore supported electrochemically in such a way that the desired thin layer forms within a short time due to the cathodic polarization provided according to the invention during the deposition process.
  • the procedure according to the invention can be implemented cost-effectively on conventional electrolytic coating systems in such a way that it can also be integrated on a large industrial scale into a continuous overall process for the production of metal sheets or strips, which are typically the case with the metallic substrates coated according to the invention.
  • the substrate to be coated according to the invention is a flat steel product.
  • the flat steel product serving as the substrate to be coated according to the invention may be provided in a manner known per se with a metallic coating, such as, for example, a Zn coating consisting of zinc or a zinc-containing alloy.
  • a time-constant potential is applied to the metal surface to be coated, and in the case of galvanostatic processes, a time-constant current.
  • the metal surface is the negative pole, ie cathodically polarized.
  • the height of the potential or the current density is individually adapted to the liquid electrolyte used.
  • the electrolyte resistance, competing electrode reactions or side reactions, the temperature of the electrolyte, the speed of the moving substrate and the electrical conductivity of the substrate surface are taken into account.
  • Suitable electrolytes for the purposes according to the invention are, for example, electrolytes from the group of aqueous and acidic electrolyte solutions.
  • suitable electrical potentials are at least 100 mV more negative than the resting or corrosion potential of the substrate surface in the electrolyte used (cathodic polarization), or a voltage of the order 1 V - 30 V voltage between the substrate (Cathode) and the circuit closing inert counter electrode (eg dimensionally stable anode).
  • suitable current densities are in the order of 0.1 mA / cm 2 - 500 mA / cm 2 between the substrate (cathode) and the circuit closing inert counter electrode (eg dimensionally stable anode).
  • the speeds at which the electrically conductive substrate is moved through the electrolyte may be in the range of 0.5-15 m / s.
  • a defined layer thickness of the conversion layer can be applied accurately and reproducibly via potential level or current density.
  • the substrate can be electrochemically pre-cleaned in a step preceding the steps carried out according to the invention.
  • the thin coating applied according to the invention can assume the dual function of "corrosion protection / adhesion promoter" as the conversion layer.
  • the inorganic coating formed according to the invention so that in each case only one or the other function is in the foreground, so that the coating essentially only to improve the adhesion or only to improve the corrosion protection contributes.
  • the invention is particularly suitable for depositing a ZrO 2 -based thin film.
  • the electrolyte used is an aqueous solution containing a Zr or Ti compound which dissociates into zirconium or titanium fluoro complexes.
  • the reaction mechanism of the ZrO 2 deposition is based on an alkalization of the metallic surface to be coated, which precipitates out of the conversion solution ZrO 2 .
  • the following reactions take place at the interface metal substrate
  • the alkalization is accelerated by cathodic polarization of the surface to be coated (Eq. (2) and (3)).
  • the ZrO 2 precipitation is forced.
  • the polarization can either take place moderately on the one hand, ie with relatively weak cathodic polarization, in which essentially the oxygen conversion takes place in the sense of an oxygen-consuming cathode (equation (3)).
  • the polarization can be carried out in such a way that mainly a hydrogen evolution (Eq. (2)) starts.
  • a suitable process window must be chosen, since a too weak polarization is not sufficiently accelerated alkalization and too strong a polarization counterproductive for the layer formation, due to the evolution of hydrogen, which leads to a Swirling or convection of the electrolyte leads and also occupied the surface to be coated with gas bubbles. Therefore, according to the invention, the process window is set in the manner already explained above.
  • Typical thicknesses of the inorganic layers deposited on the respective metallic substrate according to the invention are in the range from 20 to 200 nm.
  • sheet metal samples have been provided from a typical automotive deep-drawing steel, which is suitable by its property profile particularly for the manufacture of components for the outer skin of automobiles.
  • a deep-drawing steel of this type is known under the name HC180B (material number 1.0395).
  • the sheet metal samples have been divided from both sides galvanized and tempered steel strip to protect against corrosion in a hot dip galvanizing process.
  • the zinc layer thickness was on average 10 ⁇ m in the samples.
  • Such zinc coatings are also known in the art under the abbreviation "Z100".
  • the sheet samples may also be provided with a zinc-magnesium coating.
  • the sheet samples were pre-degreased with an alkaline detergent and neutralized by rinsing with water. Subsequently, the cleaned surface has been dried in the heated air stream.
  • each a device 1 of in Fig. 4 been shown schematically type used. Devices constructed according to this principle have hitherto been used, for example, for electrolytic belt cleaning.
  • the apparatus 1 comprises a plurality of so-called horizontal cells 2, 3, 4, each traversed in the conveying direction F, each having a basin 5, which is filled with the above-described aqueous solution as electrolyte, and through which the sheet sample P to be coated is oriented in a horizontal orientation is encouraged.
  • the electrolyte is conveyed by a pump 6 in circulation and applied via nozzles 7 in a conventional manner so on the top and bottom of the sheet sample P, that the exiting electrolyte flow flows over a large area on the relevant side of the sheet sample P.
  • Each of the roller pairs comprises a current roller 8, 9 arranged above the conveying path of the sheet metal sample P and a pressure roller 10, 11 arranged below the conveying path, which presses the sheet metal sample P against the associated current roller 8, 9.
  • the power rollers 8,9 are connected to the negative pole (-) of a rectifier / power supply unit 12 whose positive pole (+) is connected via bus bars 13 with anodes 14, which are above and below the conveying path between the power rollers / pressure roller pairs 8,10; 9.11 extend.
  • the polarization according to the invention can also be carried out in an electrically sufficiently dense spray curtain or in a suitably designed roller coating process, in which case a downstream exhaust zone or directly connected drying in a heating section with heated air or IR drying support can be provided, so that the drying at 90 ° C +/- 10 ° C within 1 - 10 seconds.
  • the sheet samples P may be coated with a non-corrosive protective oil or with a formability-promoting agent having a typical coating weight of typically up to 1.2 g / m 2 .
  • the conversion layer according to the invention also allows overlay weights significantly below this limit value, so that the protective oil or the formability-improving agent can, if necessary, be removed particularly easily for further processing from the respective sample or the component formed therefrom.
  • the sheets or strips obtained from the above-described manner according to the invention are converted into the respective component with which the vehicle body is then formed.
  • the outer coating is applied, whose adhesion to the steel substrate is ensured by the conversion layer applied in accordance with the invention.
  • a sample P provided in the manner already explained above was also pre-degreased with an alkaline detergent and neutralized by water rinse. The cleaned surface was then dried in the heated air stream.
  • the achievable fatiguenGermanskonvertierende assignment is by application of a predominantly aqueous formulation in the dipping process (with 15 sec direct dipping time) with subsequent exhaust time of up to 30 sec at room temperature and optionally subsequent forced drying in, for example, heated to 140 ° C convection oven dried.
  • a temperature increase of the first drying step up to 90 ° C compensates for increased belt speeds.
  • the applied conversion solution contained as a predominantly aqueous formulation Zr resulting from the H 2 ZrF 6 content of 0.003 mol / l to 0.1 mol / l of the conversion solution or in combination with 1 to 1.5 wt .-% organosilane resulting from the combined Epoxy-silicones containing epoxy groups.
  • the electrolyte system has been adjusted to a pH range of 4-5.5, in particular 4-4.2. This pH range has been stabilized by the addition of ammonium bicarbonate or another buffer system known in the art.
  • an electrical conductivity of the application electrolyte of 2000 +/- 500 mS / m, which is adjusted by a supporting electrolyte, and an electrode distance of 30 mm +/- 10 mm has been used.
  • the pre-cleaned sample was additionally polarized by 400 +/- 100 mV more positive relative to the rest potential for 2..5 s.
  • the method according to the invention is in particular for the application of layers of the German patent application already mentioned in the introduction, incorporated by reference into the disclosure of the present application 10 2013 113 731.8 dated December 9, 2013 and International Patent Application PCT / EP2014 / 076987 suitable.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electroplating Methods And Accessories (AREA)
EP15171740.2A 2015-06-11 2015-06-11 Procédé de séparation électrochimique de couches anorganiques minces Withdrawn EP3103897A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP15171740.2A EP3103897A1 (fr) 2015-06-11 2015-06-11 Procédé de séparation électrochimique de couches anorganiques minces

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EP15171740.2A EP3103897A1 (fr) 2015-06-11 2015-06-11 Procédé de séparation électrochimique de couches anorganiques minces

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EP3103897A1 true EP3103897A1 (fr) 2016-12-14

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010046392A2 (fr) 2008-10-23 2010-04-29 Happy Plating Gmbh Procédé d'application de revêtement par voie électrochimique
US7959982B2 (en) 2003-12-17 2011-06-14 Centre de Recherches Metallurgiques ASBL—Centrum Voor Research in de Metallurgie VZW Method for coating a metal surface with an ultrafine layer
US20110259756A1 (en) * 2010-04-22 2011-10-27 Shigeru Hirano Method of production of chemically treated steel sheet
US20110300402A1 (en) * 2010-06-04 2011-12-08 Akira Tachiki Steel sheet for container use and method of production of same
EP2439310A1 (fr) * 2009-06-04 2012-04-11 Nippon Steel Corporation Feuille d'acier pour contenants qui présente d'excellentes performances pour les couches organiques et son procédé de fabrication
US20120183753A1 (en) * 2011-01-18 2012-07-19 Shigeru Hirano Steel sheet for container having excellent organic film performance and process for producing the same
US20130206285A1 (en) * 2010-09-15 2013-08-15 Jfe Steel Corporation Manufacturing method for steel sheets for containers
US20130216858A1 (en) * 2010-09-15 2013-08-22 Jfe Steel Corporation Steel sheet for containers and manufacturing method for same
EP2787102A1 (fr) * 2011-11-30 2014-10-08 Nihon Parkerizing Co., Ltd. Supplément et procédé de production de tôle en acier traitée en surface

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7959982B2 (en) 2003-12-17 2011-06-14 Centre de Recherches Metallurgiques ASBL—Centrum Voor Research in de Metallurgie VZW Method for coating a metal surface with an ultrafine layer
EP1694879B1 (fr) 2003-12-17 2014-05-21 CENTRE DE RECHERCHES METALLURGIQUES asbl - CENTRUM VOOR RESEARCH IN DE METALLURGIE vzw Procede de revetement d une surface metallique par une couch e ultrafine
WO2010046392A2 (fr) 2008-10-23 2010-04-29 Happy Plating Gmbh Procédé d'application de revêtement par voie électrochimique
EP2439310A1 (fr) * 2009-06-04 2012-04-11 Nippon Steel Corporation Feuille d'acier pour contenants qui présente d'excellentes performances pour les couches organiques et son procédé de fabrication
US20110259756A1 (en) * 2010-04-22 2011-10-27 Shigeru Hirano Method of production of chemically treated steel sheet
US20110300402A1 (en) * 2010-06-04 2011-12-08 Akira Tachiki Steel sheet for container use and method of production of same
US20130206285A1 (en) * 2010-09-15 2013-08-15 Jfe Steel Corporation Manufacturing method for steel sheets for containers
US20130216858A1 (en) * 2010-09-15 2013-08-22 Jfe Steel Corporation Steel sheet for containers and manufacturing method for same
US20120183753A1 (en) * 2011-01-18 2012-07-19 Shigeru Hirano Steel sheet for container having excellent organic film performance and process for producing the same
EP2787102A1 (fr) * 2011-11-30 2014-10-08 Nihon Parkerizing Co., Ltd. Supplément et procédé de production de tôle en acier traitée en surface

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
KORYTA, J.; DVORAK, J.; BOHACKOVA, V: "Lehrbuch der Elektrochemie", 1975, SPRINGER VERLAG, pages: XVI
P. PUOMI; H. M. FAGERHOLM; J. B. ROSENHOLM; K. JYRKÄS: "Comparison of different commercial pretreatment methods for hot-dip galvanized and galfan coated steel", SURFACE AND COATINGS TECHNOLOGY, vol. 115, 1999, pages 70 - 78, XP027295423
P. PUOMI; H. M. FAGERHOLM; J. B. ROSENHOLM; R. SIPILÄ: "Optimization of commercial zirconic acid based pretreatment on hot-dip galvanized and galfan coated steel", SURFACE AND COATINGS TECHNOLOGY, vol. 115, 1999, pages 79 - 86, XP027295424
T. LOSTAK; A. MALJUSCH; B. KLINK; S. KREBS; M. KIMPEL; J. FLOCK; S. SCHULZ; W. SCHUHMANN: "Zr-based conversion layer on Zn-Al-Mg alloy coated steel sheets: insights into the formation mechanism", ELECTROCHIMICA ACTA, vol. 137, 2014, pages 65 - 74
T. LOSTAK; S. KREBS; A. MALJUSCH; T. GOTHE; M. GIZA; M. KIMPEL; J. FLOCK; S. SCHULZ: "Formation and characterization of Fe3+- / Cu2+-modified zirconium oxide conversion layers on zinc alloy coated steel sheets", ELECTROCHIMICA ACTA, vol. 112, 2013, pages 14 - 23, XP028789661, DOI: doi:10.1016/j.electacta.2013.08.161

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