US20060193988A1 - Method for coating metallic surfaces with a mixture containing at least two silanes - Google Patents

Method for coating metallic surfaces with a mixture containing at least two silanes Download PDF

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Publication number
US20060193988A1
US20060193988A1 US10/546,624 US54662405A US2006193988A1 US 20060193988 A1 US20060193988 A1 US 20060193988A1 US 54662405 A US54662405 A US 54662405A US 2006193988 A1 US2006193988 A1 US 2006193988A1
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United States
Prior art keywords
silane
process according
group
fluorine
aqueous composition
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US10/546,624
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English (en)
Inventor
Manfred Walter
Axel Schone
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CHEMETAL GmbH
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CHEMETAL GmbH
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=32928840&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=US20060193988(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Priority claimed from DE10308237.9A external-priority patent/DE10308237B4/de
Priority claimed from DE10332744.4A external-priority patent/DE10332744B4/de
Application filed by CHEMETAL GmbH filed Critical CHEMETAL GmbH
Assigned to CHEMETAL GMBH reassignment CHEMETAL GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BROWN, KEVIN, JUNG, CHRISTIAN, KLIEHM, NORBERT, SCHONE, AXEL, WALTER, MANFRED, KOLBERG, THOMAS
Publication of US20060193988A1 publication Critical patent/US20060193988A1/en
Priority to US12/958,009 priority Critical patent/US8932679B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C09D175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • 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
    • 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
    • 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
    • C23C22/60—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 alkaline aqueous solutions with pH greater than 8
    • 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
    • C23C22/68—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 solutions with pH between 6 and 8
    • 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
    • C23C22/73—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 characterised by the process
    • C23C22/74—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 characterised by the process for obtaining burned-in conversion coatings
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C23C22/83—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0091—Complexes with metal-heteroatom-bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
    • 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
    • C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/20—Use of solutions containing silanes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31652—Of asbestos
    • Y10T428/31663—As siloxane, silicone or silane

Definitions

  • the invention relates to a process for coating metallic surfaces with an aqueous composition comprising at least one fluorine-free silane and at least one fluorine-containing silane and, if desired, organic film formers and/or further components.
  • the invention further relates to such aqueous compositions and also to the use of the substrates coated by the process of the invention.
  • silanes in aqueous compositions for producing siloxane-rich corrosion-protective coatings is known in principle. Although these coatings have become established, the processes for coating with an aqueous composition predominantly comprising silane are in some cases difficult to implement. This coating is not always formed with ideal properties. In addition there may be problems in the ability sufficiently to characterize the very thin, transparent silane coatings on the metallic substrate, and defects therein, with the naked eye or with optical aids. Corrosion protection and film adhesion of the siloxane-rich coatings formed are often high, though not always so, and in some cases are not high enough for certain applications even when the coatings are appropriately applied.
  • silane-containing aqueous compositions In the context of the design of silane-containing aqueous compositions, moreover, it has been found appropriate to add a small or large amount of at least one component selected from the group consisting of monomers, oligomers and polymers. With compositions of this kind the nature and amount of the silane added are sometimes critical to a successful outcome. Normally, however, the amounts of silane added for the purpose are comparatively low—often only up to 5% by weight—and in that case act as a coupling agent, where the intention is that it is the adhesion-promoting (coupling) effect in particular between the metallic substrate and coating material and, where appropriate, between pigment and organic coating-material constituents that should prevail, although to a minor extent in some cases there may also be a slight crosslinking effect. Additions of silane are made predominantly to thermally curable resin systems.
  • WO 00/46310 teaches a process for coating metallic surfaces with a liquid composition which comprises a hydrolyzed aminosilane and a hydrolyzed multi-silyl-functional silane, but no fluorine-containing silane.
  • DE-A1-101 49 148 describes aqueous coating compositions based on organic film former, fine inorganic particles and also lubricants and/or organic corrosion inhibitor, the compositions providing outstanding results in corrosion resistance, adhesion and formability, not least on Galvalume® steel sheets, despite the absence of chromium compounds, but nevertheless also exhibiting inadequate corrosion resistance as an organic film approximately 1 ⁇ m thick on hot-dip-galvanized, electrolytically galvanized or Galfan®-coated metallic strips, i.e. on metallic surfaces which are difficult to protect against corrosion.
  • the compositions, their constituents and the properties of the raw materials and coatings in that publication are expressly incorporated by reference into this specification.
  • German patent application DE 103 08 237 of 25.02.2003 relating to compositions of similar constitution and to corresponding processes for coating metallic surfaces, is explicitly incorporated by reference in terms of the raw materials and their properties, the preparation of the compositions and/or the hydrolyzing of the silanes, the compositions such as concentrates and baths and their properties, the effects, the formation of the coatings such as the drying, filming and curing, for example, the compositions and the properties of the coatings formed, and also the variants of the processes.
  • the object is achieved with a process for coating a metallic surface, in particular of aluminum, iron, copper, magnesium, nickel, titanium, tin, zinc or alloys containing aluminum, iron, copper, magnesium, nickel, titanium, tin and/or zinc, with an aqueous composition, also comprising, if desired, organic solvent and other components, which is substantially or entirely free from chromium(VI) compounds, for the purpose of pretreatment prior to a further coating or for treatment, where the article to be coated—in particular a strip or strip section—is, if desired, formed after coating, which process is characterized in that the composition comprises, besides water,
  • the silanes in the composition being water-soluble or becoming water-soluble in particular by virtue of (further) hydrolysis reactions and/or chemical reactions prior to application to the metallic surface,
  • the clean, pickled, cleaned and/or pretreated metallic surface being contacted with the aqueous composition and a film being formed on the metallic surface and subsequently dried and, if desired, additionally cured,
  • the object is also achieved by aqueous compositions corresponding to claim 26 .
  • the silane is characterized in this specification by the dominant constituent of the products, which are generally available commercially.
  • the silanes present in the aqueous composition are monomers, oligomers, polymers, copolymers and/or reaction products with further components as a result of hydrolysis reactions, condensation reactions and/or further reactions. The reactions take place primarily in solution, in the course of the drying and, where appropriate, curing of the coating.
  • the term “silane” is utilized in this context for silanes, silanols, siloxanes, polysiloxanes and their reaction products and/or derivatives, which are often “silane” mixtures. In view of the often highly complex chemical reactions which occur in this context, and in view of highly complex analyses and operations, it is not possible to specify the particular further silanes and other reaction products.
  • silanes for the purposes of this specification are regarded as being water-soluble if they summarily at room temperature in the silane composition have a solubility in water of at least 0.05 g/l, preferably at least 0.1 g/l, more preferably at least 0.2 g/l or at least 0.3 g/l. This does not imply that every single one of these silanes must have this minimum solubility but rather that these minimum values are achieved on average.
  • aqueous composition preferably there is at least one silane selected from the fluorine-free silanes: from in each case at least one acyloxysilane, alkoxysilane, silane having at least one amino group such as an aminoalkylsilane, silane having at least one succinic acid group and/or succinic anhydride group, bis-silyl-silane, silane having at least one epoxy group such as a glycidyloxysilane, (meth)acrylato-silane, multi-silyl-silane, ureidosilane, vinylsilane and/or at least one silanol and/or at least one siloxane or polysiloxane whose composition corresponds chemically to that of the aforementioned silanes.
  • silane selected from the fluorine-free silanes: from in each case at least one acyloxysilane, alkoxysilane, silane having at least one amino group such as an aminoalkylsi
  • It comprises at least one silane and/or (in each case) at least one monomeric, dimeric, oligomeric and/or polymeric silanol and/or (in each case) at least one monomeric, dimeric, oligomeric and/or polymeric siloxane, the term “oligomers” being intended here to embrace even trimers.
  • the aqueous composition there is at least one silane selected from the fluorine-containing silanes: from in each case at least one acyloxysilane, alkoxysilane, silane having at least one amino group such as an aminoalkylsilane, silane having at least one succinic acid group and/or succinic anhydride group, bis-silyl-silane, silane having at least one epoxy group such as a glycidyloxysilane, (meth)acrylato-silane, multi-silyl-silane, ureidosilane, vinylsilane and/or at least one silanol and/or at least one siloxane or polysiloxane whose composition corresponds chemically to that of the aforementioned silanes, containing in each case at least one group that contains one, or contains at least one, fluorine atom.
  • silane selected from the fluorine-containing silanes: from in each case at least one acyloxysilane,
  • the aqueous composition comprises at least one fluoroalkoxyalkylsilane, at least one mono-, di- or trifunctional fluorosilane, at least one mono-, bis- or tris-fluorosilane, at least one fluorosilane based on ethoxysilane and/or based on methoxysilane and/or at least one fluorosilane having at least one functional group such as, for example, an amino group, in particular in the form of a cocondensate, such as, for example, a fluoroalkyldialkoxysilane, a fluoroaminoalkylpropyltrialkoxysilane, a fluoromethanesulfonate, a fluoropropylalkyldialkoxysilane, a triphenylfluorosilane, a trialkoxyfluorosilane, a trialkylfluorosilane and/or a tridecafluorooctylt
  • composition comprises at least one silane that contains at least two amino groups and also at least one ethyl group and/or at least one methyl group.
  • the amount of all silanes a) and b), including any reaction products formed with other components is together preferably from 0.01 to 100 g/l in a concentrate or from 0.002 to 12 g/l in a bath. In the case of a concentrate this amount is more preferably in the range from 0.05 to 80 g/l, very preferably in the range from 0.1 to 60 g/l, in particular roughly 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 20, 22.5, 25, 27.5, 30, 35, 40, 45, 50 or 55 g/l.
  • this amount is more preferably in the range from 0.005 to 5 g/l, very preferably in the range from 0.01 to 3 g/l, in particular roughly 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 2.0, 2.25, 2.5 or 2.75 g/l.
  • Dilution of the concentrate which is normally carried out with water and only occasionally with a mixture of water and at least one organic solvent, can be carried out in particular by a factor of from 1.5 to 30, frequently by a factor of from 2 to 20, in particular by a factor of from 3 to 12.
  • the proportion of a) to b) is preferably in each case in the range from 1:0.01 to 1:4, more preferably in a proportion of from 1:0.03 to 1:3, very preferably in a proportion of from 1:0.05 to 1:2.5 and in particular is in each case at least 1:0.08, 1:0.12, 1:0.16, 1:0.2, 1:0.25, 1:0.3, 1:0.35, 1:0.4, 1:0.45 or 1:0.5 or in particular in each case up to 1:2.5, 1:2.2, 1:2, 1:1.8, 1:1.6, 1:1.4, 1:1.2, 1:1.1, 1:1, 1:0.9, 1:0.8, 1:0.7 or 1:0.6.
  • the particular optimum of this proportion may fluctuate, however, according to which silanes a) and b) are used and how they are hydrolyzed.
  • an aqueous composition is selected on the criteria that more than 60% by weight, in particular more than 80% by weight of the silanes have good water-solubility and that the composition prepared therewith in the form of a concentrate or bath possesses good stability for the time of processing. This processing time may vary between 2 hours and 6 months according to requirements. Good stability here means that the composition undergoes only slight precipitation, if any at all, and only slight chemical and/or physical change, if any at all.
  • the composition composed essentially of silanes and solvents is preferably clear. In this context it is preferred to select those silanes and those reactions and process steps such that the compounds formed from the silanes in such reactions/steps adopt structures which can be regarded as ladder structures to a relatively large extent, in particular predominantly or even extensively.
  • At least two different fluorine-free silanes can be particularly preferable to add at least two different fluorine-free silanes, possibly even three or four different fluorine-free silanes, to the aqueous composition.
  • Particular preference is given to a combination of in each case at least one organosilane, one organo-functional silane and one fluoro-silane, in particular of in each case at least one aminosilane, one multi-silyl-silane and one fluoro-silane.
  • the aqueous composition which in this specification is referred to as a solution, need not be a solution in the strict sense, especially since it is often possible only by means of additional analyses to determine whether the solutions in question are true solutions.
  • the aqueous composition may also be a suspension and/or emulsion, especially when particles, particularly inorganic particles, are added.
  • the aqueous composition comprises as solvent at least water, the water content in the solvent mixture being more than 50% by weight in the case of a concentrate and more than 75% by weight in the case of a bath composition.
  • the amount of water in the solvent mixture in the case of a concentrate is preferably at least 60% by weight, more preferably at least 70% by weight, very preferably at least 80% by weight, in particular at least 90% by weight.
  • the amount of water in the solvent mixture in the case of a bath composition is preferably at least 80% by weight, more preferably at least 85% by weight, very preferably at least 90% by weight, in particular at least 95% by weight.
  • the amount of further solvents other than water in other words particularly of organic solvents such as ethanol, methanol, propanol and/or isopropanol, for example, may on the one hand be added to the concentrate or to the bath and/or may be formed in the concentrate or bath by chemical reactions.
  • organic solvents such as ethanol, methanol, propanol and/or isopropanol
  • a certain organic solvent content or low organic solvent content is sometimes preferred, but in some cases, owing to chemical reactions, it is unavoidable unless the organic solvent is removed artificially afterwards.
  • the aqueous composition contains not more than 0.2 g/l chromium, preferably not more than 0.1 g/l chromium, more preferably not more than 0.02 g/l chromium, the chromium content possibly originating in particular from entrainments and/or from etching operations on chromium-containing alloys and/or chrome plating. Preferably there are also no contents of further heavy metals, besides iron, manganese and zinc, that total more than 0.8 g/l.
  • the aqueous composition comprises the silanes a) and b), water and, if desired, at least one organic solvent such as methanol, ethanol, isopropanol and/or propanol, for example, at least one alkaline agent such as ammonia, for example, at least one acidic agent such as acetic acid and/or glacial acetic acid, for example, at least one surfactant to reduce the surface tension and for uniformly and reliably coating the metallic surface, such as at least one nonionic, at least one anionic, at least one cationic and/or at least one amphoteric surfactant, for example, and/or at least one additive such as at least one preservative and/or at least one biocide, for example.
  • at least one organic solvent such as methanol, ethanol, isopropanol and/or propanol
  • at least one alkaline agent such as ammonia
  • at least one acidic agent such as acetic acid and/or glacial acetic acid
  • the bath compositions of the aqueous compositions predominantly comprising silanes preferably have a water content in the range from 80 to 99.9% by weight, more preferably in the range from 90 to 99.8% by weight, very preferably in the range from 94 to 99.7% by weight, particularly in the range from 96 to 99.6% by weight, in particular about 91, 91.5, 92, 92.5, 93, 93.5, 94, 94.5, 95, 95.5, 96, 96.5, 97, 97.5, 97.9, 98.2, 98.5, 98.8, 99.1 or 99.4% by weight.
  • the amounts of further components besides silanes and solvents in the bath are normally not more than 5 g/l in total, preferably not more than 3 g/l in total, more preferably not more than 1.5 g/l, but in the concentrate may be higher accordingly.
  • amounts of chelate(s), in each case including the resultant reaction products of from 0.01 to 15% by weight, based on the solids content of the bath composition, more preferably, in each case independently of one another, amounts of from 0.03 to 11% by weight, in particular roughly amounts, independently of one another in each case, of 0.05, 0.1, 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10 or 10.5% by weight.
  • At least one silane is selected that is compatible with water, i.e. such that the at least one silane and/or, where appropriate, its hydrolysis and condensation products are miscible with the components of the aqueous composition, without disruption, and have a keeping duration of at least several weeks, and that it allows the formation of a defect-free wet film and dry film which in particular is coherent, uniform and free from craters.
  • Selected in particular is at least one silane which enables high corrosion resistance in particular in combination with the selected, at least one chelate.
  • At least one chelate is selected which behaves stably in aqueous dispersions in the presence of the other components of the aqueous composition for a number of days or weeks and which enables a high corrosion resistance.
  • the at least one silane but also the at least one chelate are able to attach chemically to the envisaged metal surface that is to be contacted therewith and where appropriate are likewise able, to attach chemically to the coating material to be applied subsequently.
  • the at least one metal chelate is in particular one of Al, B, Ca, Fe, Hf, La, Mg, Mn, Si, Ti, Y, Zn, Zr and/or at least one lanthanide such as Ce or such as a Ce-containing lanthanide mixture, selected with particular preference from the group consisting of Al, Hf, Mn, Si, Ti, Y and Zr.
  • the concentrates of the aqueous compositions comprising predominantly silanes and also chelate(s) and also of the part-components as a starting product of polymer-containing compositions preferably have a water content in the range from 20 to 95% by weight, in particular from 30 to 90% by weight.
  • the concentrates preferably comprise the silanes, including the reaction products formed therefrom, in an amount in the range from 0.1 to 60% by weight, more preferably in the range from 0.2 to 45% by weight, very preferably in the range from 0.3 to 35% by weight, in particular in the range from 0.5 to 32% by weight, especially of about 0.8, 1, 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, 22.5, 25, 27.5 or 30% by weight, and preferably comprise the at least one chelate, including any reaction products formed therefrom, in the range from 0.1 to 50% by weight, more preferably in the range from 0.2 to 40% by weight, very preferably in the range from 0.3 to 30% by weight, in particular in the range from 0.5 to 25% by weight, especially of about 0.75, 1, 2, 4, 6, 8, 10, 12, 14, 16, 18, 20 or 22.5% by weight.
  • the bath compositions of the aqueous compositions comprising predominantly silane and chelate preferably have a water content in the range from 80 to 99.9% by weight, which may also include a fraction of at least one organic solvent.
  • the amount of water and/or at least one organic solvent is preferably in the range from 90 to 99.8% by weight, more preferably in the range from 94 to 99.7% by weight, in particular in the range from 96 to 99.6% by weight, especially of about 95, 95.5, 96, 96.5, 97, 97.5, 97.9, 98.2, 98.5, 98.8, 99.1 or 99.4% by weight.
  • the bath compositions preferably comprise the silanes, including any reaction products formed therefrom with other components, in an amount in the range from 0.01 to 10% by weight, more preferably in the range from 0.05 to 7% by weight, very preferably in the range from 0.1 to 5% by weight, in particular in the range from 0.2 to 4% by weight, especially of about 0.4, 0.6, 0.8, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.4, 2.6, 2.8, 3.0, 3.2, 3.4, 3.6 or 3.8% by weight, and preferably comprise the at least one chelate, including any reaction products formed therefrom, in the range from 0.01 to 10% by weight, more preferably in the range from 0.05 to 7% by weight, very preferably in the range from 0.1 to 5% by weight, in particular in the range from 0.2 to 4% by weight, especially of about 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9
  • the amounts of the silanes and of the at least one chelate, including in each case the reaction products formed therefrom, particularly those of titanium, hafnium and/or zirconium, preferably account for at least 20% by weight, in particular at least 30% by weight, more preferably at least 40%, very preferably at least 50% by weight, in particular in each case at least 60, 70, 80, 90, 94, 95, 96, 97, 98 or 99% by weight of the solids contents of this composition.
  • this composition is composed essentially of water, in each case at least one silane and/or reaction products thereof, at least one chelate, including any reaction products formed therefrom, and also, if desired, amounts of substances selected from the group consisting of alcohols, acids such as carboxylic acids and fatty acids such as acetic acid and/or mineral acids and other substances which influence pH, such as ammonia, and/or additives and impurities.
  • the total amount of further compounds, including additives, besides silane and chelate is normally up to 20% by weight of the solids content of silane and chelate, preferably up to 15% by weight, more preferably up to 10% by weight, very preferably up to 5% by weight, in particular up to 1 or 2% by weight.
  • the ratio of the at least one silane, including the reaction products formed therefrom, to the at least one chelate, including any reaction products formed therefrom can preferably be in the range from 0.8:1 to 1.2:1, it has surprisingly become clear that this ratio can also be in particular in the range from 0.2:1 to 0.5:1 or can be from 2:1 to 5:1, since there may be an optimum there in certain situations.
  • the pH of the bath composition can be in particular in the range from 3 to 9.5, preferably in the range from 3.5 to 9, in particular in the range from 4 to 8.8.
  • an amount of a weak acid or of a dilute strong acid, or an acid mixture In particular it is possible to use at least one acid such as carboxylic acids or fatty acids such as acetic acid and/or mineral acids and other substances which influence pH, such as ammonia.
  • the bath composition can in some cases be adjusted to pH values about 3.5 units less by addition of acid, if the chemical system withstands the chosen pH and remains stable.
  • a solvent such as an alcohol to stabilize the silane.
  • the coatings formed with these bath compositions typically have a film thickness in the range from 0.01 to 0.6 ⁇ m, generally from 0.015 to 0.25 ⁇ m.
  • the inventive composition may also comprise monomers, oligomers, polymers and/or copolymers.
  • copolymers preferably embraces block copolymers and graft copolymers as well.
  • the acid number of the synthetic resins is preferably from 3 to 100, more preferably from 3 to 60 or from 4 to 50.
  • copolymers having an acid number in the range from 3 to 50 are added to the aqueous composition.
  • the components of the organic film former that are to be added are already in partly neutralized form.
  • the organic film former may preferably include a fraction of at least one copolymer having an acid number in the range from 3 to 80, in particular to an extent of at least 50% by weight of the synthetic resins added.
  • Within a high acid-number range it is normally not necessary to stabilize a film former cationically, anionically and/or sterically. In the case of a low acid number, however, such stabilization is often necessary. In that case it is advantageous to use already (partly) stabilized synthetic resins and/or mixtures thereof.
  • the aqueous composition preferably comprises at least one synthetic resin such as organic polymer, copolymer and/or mixture thereof, in particular a synthetic resin based on acrylate, ethylene, polyester, polyurethane, silicone-polyester, epoxide, phenol, styrene, melamine-formaldehyde, urea-formaldehyde and/or vinyl.
  • synthetic resin such as organic polymer, copolymer and/or mixture thereof, in particular a synthetic resin based on acrylate, ethylene, polyester, polyurethane, silicone-polyester, epoxide, phenol, styrene, melamine-formaldehyde, urea-formaldehyde and/or vinyl.
  • the organic film former may preferably comprise a synthetic resin mixture of at least one polymer and/or at least one copolymer, comprising, in each case independently of one another, synthetic resin based on acrylate, epoxide, ethylene, urea-formaldehyde, phenol, polyester, polyurethane, styrene, styrene-butadiene and/or vinyl.
  • the film former may also be a cationically, anionically and/or sterically stabilized synthetic resin or polymer and/or a dispersion thereof or even a solution thereof.
  • acrylate includes acrylic esters, polyacrylic acid, methacrylic esters and methacrylate.
  • the organic film former may preferably comprise at least one component based on
  • the organic film former may also preferably comprise as synthetic resin an amount of organic polymer, copolymer and/or mixtures thereof based on polyethyleneimine, polyvinyl alcohol, polyvinylphenol, polyvinylpyrrolidone and/or polyaspartic acid, in particular copolymers with a phosphorus-containing vinyl compound.
  • a conductive polymer is added to the aqueous composition.
  • the weight ratio of compounds of component d)—monomers/oligomers/polymers/copolymers—to silanes in the concentrate and/or in the bath is preferably in the range from 0.1:1 to 10:1, more preferably in the range from 0.2:1 to 5:1, very preferably in the range from 0.3:1 to 3:1, and in particular is up to 2:1 or up to 1.5:1.
  • the silanes can act not only and normally only to a minor extent or not at all as a coupling agent.
  • the weight ratio of compounds of component d)—monomers/oligomers/polymers/copolymers—to silanes in the concentrate and/or in the bath is preferably in the range from 3:1 to 200:1, more preferably in the range from 8:1 to 120:1, very preferably in the range from 12:1 to 100:1.
  • the silanes in many cases act partly, predominantly or wholly only as a coupling agent.
  • a mixture of organic film formers in which at least one part of the film formers has a glass transition temperature T g of substantially equal and/or similar T g . It is particularly preferred here for at least part of the organic film formers to have a glass transition temperature T g in the range from 10 to 70° C., very preferably in the range from 15 to 65° C., in particular in the range from 20 to 60° C.
  • the organic film former then preferably comprises at least one fraction of at least one polymer and/or at least one copolymer having a minimum film formation temperature MFFT in the range from ⁇ 10 to +99° C., more preferably in the range from 0 to 90° C., in particular from 5° C.
  • the aqueous composition is admixed with synthetic resins of which at least 80% by weight have thermoplastic properties, in particular at least 90% by weight.
  • film-forming assistants in this context is not simple; often a mixture of at least two film-forming assistants is necessary.
  • Particularly advantageous film-forming assistants are what are called long-chain alcohols, particularly those having 4 to 20 carbon atoms, such as a butanediol, a butyl glycol, a butyl diglycol, an ethylene glycol ether such as ethylene glycol monobutyl ether, ethylene glycol monoethyl ether, ethylene glycol monomethyl ether, ethyl glycol propyl ether, ethylene glycol hexyl ether, diethylene glycol methyl ether, diethylene glycol ethyl ether, diethylene glycol butyl ether, diethylene glycol hexyl ether or a polypropylene glycol ether such as propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, tripropylene glycol monomethyl ether, propylene glycol monobutyl ether,
  • a hydrophobic surface which owing to the hydrophobicity and/or the surface microstructure has self-cleaning properties.
  • the surface microstructure through the addition of organic and/or inorganic particles, through formation of organic particles, through the appropriate process regime to obtain a microstructure such that as a result there is structuring in the nanometer and/or micrometer range.
  • the particles which are added preferably possess to a relatively large extent a rough surface and/or a complex geometry and/or associate and/or are associated so as to form aggregates and/or agglomerates which are of complex shape or rough to a greater extent.
  • This process may be assisted by adding particles differing in fineness: that is, particles of different average size and/or different size distribution.
  • the coating produced in this way may preferably have a surface that has a microstructure which is at least partly such that a microstructure is superimposed on a moderately fine microstructure.
  • This coating may be constituted on the basis of the compositions of the particularly preferred first, second or third variant.
  • At least one component selected from e 1 ) to e 9 ) is present and if desired at least one of components c) or d) is also present, in addition, if desired, to at least one monomer/oligomer/polymer/copolymer and/or to at least one inorganic compound in particle form.
  • lubricant e 2 it is preferred as lubricant e 2 ) to use at least one wax selected from the group consisting of paraffins, polyethylenes and polypropylenes, in particular an oxidized wax, the amount of waxes in the aqueous composition being preferably in the range from 0.01 to 5% by weight, more preferably in the range from 0.02 to 3.5% by weight, very preferably in the range from 0.05 to 2% by weight.
  • the melting point of the wax used as lubricant is preferably in the range from 40 to 165° C., more preferably in the range from 50 to 160° C., and in particular in the range from 120 to 150° C.
  • a lubricant having a melting point in the range from 120 to 165° C. it is particularly advantageous, in addition to a lubricant having a melting point in the range from 120 to 165° C., to add a lubricant having a melting point in the range from 45 to 95° C. or having a glass transition temperature in the range from ⁇ 20° C. to +60° C., in particular in amounts of from 2 to 30% by weight, preferably from 5 to 20% by weight, of the total solids content.
  • This latter lubricant may also be used with advantage alone.
  • the wax in the form of an aqueous dispersion and/or a cationically, anionically and/or sterically stabilized dispersion, since it can then be maintained in homogeneously distributed form in the aqueous composition with ease.
  • the at least one lubricant which if desired may also at the same time be a forming agent, is preferably present in an amount in the range from 0.1 to 25 g/l and more preferably in an amount in the range from 1 to 15 g/l in the aqueous composition.
  • the aqueous composition preferably comprises at least one organic corrosion inhibitor e 3 ), based in particular on amine(s), preferably at least one alkanolamine—preferably a long-chain alkanolamine, at least one TPA-amine complex such as acid adduct-4-oxo-4-p-tolyl butyrate-4-ethylmorpholine, at least one zinc salt of aminocarboxylate, of 5-nitro-isophthalic acid or of cyanic acid, at least one polymeric ammonium salt with fatty acid, at least one metal salt of a sulfonic acid such as dodecyl-naphthalenesulfonic acid, at least one amino complex and transition metal complex of toluenepropionic acid, 2-mercapto-benzothiazolyl-succinic acid and/or of at least one of their amino salts, at least one conductive polymer and/or at least one thiol, it being possible for the amount of organic corrosion inhibitors in the aqueous composition
  • the at least one organic corrosion inhibitor is preferably not highly volatile at room temperature. Further, it may be advantageous if it is readily soluble in water and/or readily dispersible in water, in particular at more than 20 g/l. Particular preference is given, inter alia, to alkylaminoethanols such as dimethylaminoethanol and/or complexes based on a TPA amine such as N-ethylmorpholine complex with 4-methyl- ⁇ -oxo-benzenebutanoic acid. This corrosion inhibitor can be added in order to produce greater corrosion inhibition or to make corrosion inhibition even greater.
  • the aqueous composition preferably contains from 0.1 to 80 g/l of the at least one anti-corrosion pigment e 4 ).
  • these include, in particular, various silicates based on aluminum silicates, aluminosilicates, alumino-alkaline-earth metal silicates, and alkaline-earth metal silicates.
  • the anti-corrosion pigments preferably have an average particle diameter, measured on a scanning electron microscope, in the range from 0.01 to 0.5 ⁇ m diameter, in particular in the range from 0.02 to 0.3 ⁇ m.
  • the various kinds of anti-corrosion pigments are known in principle. An addition of at least one of these pigments, however, does not appear fundamentally to be necessary, but makes alternative variants possible.
  • the agents for neutralizing and/or sterically stabilizing the acid groups of the synthetic resins with an acid number in particular in the range from 5 to 50, e 5 ), may be, inter alia, low-volatility alkanolamines and hydroxides such as sodium hydroxide and potassium hydroxide solutions, but preferably high-volatility alkanolamines, ammonia and compounds based on morpholine and alkanolamines. Their effect is that the neutralized synthetic resins become miscible with water and/or are even soluble in water in the case of an acid number of about 150 or more.
  • organic solvent e 6 it is also possible if desired to add at least one organic solvent e 6 ).
  • organic solvent for the organic polymers it is possible to use at least one water-miscible and/or water-soluble alcohol, a glycol ether or n-methylpyrrolidone and/or water; where a solvent mixture is used it is possible in particular to use a mixture of at least one long-chain alcohol, such as propylene glycol, an ester alcohol, a glycol ether and/or butanediol, for example, with water. In many cases, however, it is preferred to add only water without any organic solvent at all.
  • organic solvent its amount is preferably from 0.1 to 10% by weight, in particular from 0.25 to 5% by weight, very preferably from 0.4 to 3% by weight.
  • organic solvent for strip production it is preferred to use, rather, only water and almost no organic solvents or none at all, apart possibly from small amounts of alcohol.
  • wetting agent in order to allow the wet film to be applied uniformly in its two-dimensional extent and in film thickness and also to allow it to be applied coherently and with no defects.
  • wetting agents are suitable for this purpose, preferably acrylates, silanes, polysiloxanes, and long-chain alcohols, which lower the surface tension of the aqueous composition.
  • Particular preference is given to adding at least one polysiloxane e 7 ).
  • the addition of at least one surfactant e 9 may help to improve the wetting of the composition of the invention on a metallic surface and to improve the coating, in particular to make it more uniform.
  • a distinct improvement can be achieved in particular in the case of surfaces which are particularly rough.
  • Suitability for this purpose is possessed by a very large number of kinds of surfactants, particularly nonionic, cationic, amphoteric and anionic surfactants.
  • a low level of addition in the range from 0.01 to 0.4 g/l is often sufficient.
  • compositions of the invention can, furthermore, also be used as an after-rinse solution, following a prior coating operation such as, for example, a conversion coating operation.
  • a conversion coating it is possible, for example, to apply coatings based on at least one organic and/or inorganic acid, if desired with further adjuvants, based on a phosphating treatment, for example on the basis of iron, calcium, magnesium, manganese and/or zinc, produced on the basis of a complex fluoride-containing solution or dispersion, based on phosphonate, based on at least one silane/siloxane and/or polysiloxane and/or based on rare earth compounds, to the metallic surfaces first of all.
  • Such solutions or after-rinse solutions may therefore be particularly suitable for bright corrosion protection, where no paint and no paint-like coatings are applied.
  • a conversion coating based on rare earth compounds such as cerium oxide, for example, can be employed in particular on surfaces rich in Al, Mg, Ti and/or Zn.
  • aqueous concentrates an aqueous mixture in accordance with table 1 was prepared for the silanes which were not yet prehydrolyzed, the said mixture already containing the glacial acetic acid and ethanol, by prehydrolyzing at least one silane in acidic medium for at least three days at room temperature with stirring, where the silanes to be used were not already in prehydrolyzed form. Thereafter the silane already in prehydrolyzed form, where appropriate, was added, the system was stirred intensively and the preparation was stored at room temperature where appropriate. Thereafter the concentrates were diluted with water and, if desired, a pH modifier such as ammonia and/or glacial acetic acid was added in order to obtain treatment baths ready for use.
  • a pH modifier such as ammonia and/or glacial acetic acid was added in order to obtain treatment baths ready for use.
  • Silanes A and B are fluorine-free, silane C is fluorine-containing.
  • Silane A is an amino-functional trialkoxysilane which was hydrolyzed for only about two hours before being added to the composition.
  • Silane B is a bis-trialkoxysilane which was hydrolyzed and stored for about three days before being added to the composition.
  • Silane C is a water-soluble aminoalkyl-functional fluoroalkylalkoxysilane which was added to the composition only after a very long time of hydrolysis and of storage.
  • the silanes present in the aqueous composition are monomers, oligomers, polymers, copolymers and/or reaction products with further components owing to hydrolysis reactions, condensation reactions and/or other reactions. The reactions take place primarily in the solution, during drying and, where appropriate, curing of the coating.
  • silane is used here for silanes, silanols, siloxanes, polysiloxanes and their reaction products and derivatives, which are often “silane” mixtures. All of the concentrates and baths proved to be stable for one week without changes or precipitation. No ethanol was added. Amounts of ethanol in the compositions originated only from chemical reactions.
  • Polymer D is a readily filming thermoplastic polymer based on ethoxylate.
  • Polymer E is a polyethylene copolymer.
  • the SiO 2 particles had an average size of approximately 200 nm.
  • Monoethanolamine and/or ammonia were added to the bath in order to adapt the pH.
  • an amount of approximately 0.1 g/l of nonionic surfactant was added in each case. This addition of surfactant helped in more effective wetting of the cleaned metallic surface. As a result, more uniform film formation was obtained, particularly in the case of metallic surfaces of relatively complex shape or of particular roughness. Using these compositions, a coating with a dry film thickness of significantly less than 1 ⁇ m was produced.
  • compositions of high silane content amounts in g/l for concentrates; remainder water Inventive/comparative examples CE CE CE IE IE IE IE CE CE CE IE IE IE 1 2 3 4 5 6 7 8 9 10 11 12 13 Organo- 46 — 46 23 46 59 — — — 92 92 92 92 functional silane A Organosilane B — 95 95 48 95 122 — — — 190 190 190 F-silane C — — — — 4.3 8.5 1.7 4.3 8.5 17 — 17 34 102 Polymer D — — — — — — — — — — — — — — Polymer E — — — — — — — — — — — — — — SiO 2 particles — — — — — — — — — — — — — — — — — Glacial acetic 0.5
  • the films formed here were transparent, uniform and coherent. In all cases apart from CE 2, they showed no coloring on steel sheet. The structure, gloss and color of the metallic surface appeared to be changed only a little as a result of the coating.
  • the corrosion protection values run from 0 to 5, with 5 representing the poorest values.
  • the selection of the systems composed of fluorine-free silanes and/or of fluorine-containing silane showed its worth, since all of these combinations gave very stable solutions.
  • the contact angle was measured using a DIGIDROP Contact Angle Meter from GBX Scientific Instruments using double-distilled water over 5 measurements per sheet. The greater the contact angles, the more hydrophobic the surface. In the case of experiment CE 2, in contradistinction to the other coated sheets, the steel sheet coated showed the color of golden rust, which had an adverse effect on the contact angle. Additionally it was found that the contact angle was determined not only by the silane applied, alone, but also by the effects of the surface treatment, such as the pH, for example. It emerged, surprisingly, that in the case of these experiments an remarkably strict correlation occurred between the hydrophobicity of the coated surface, the contact angle, and the corrosion resistance of the coating system.
  • the coatings produced herewith are in many cases suitable for coating with powder coating material or with solvent-based paint. Water-based paint compositions, in contrast, are repelled.
  • aqueous solutions were prepared as in the case of experiment series A), with the exceptions that the compositions were chosen in accordance with table 3 and the conversion-coated metal sheets based on the aluminum alloy AA 6063 were coated by being immersed in the bath solution for 1 minute at room temperature.
  • the thicknesses of the coating of the invention produced with the after-rinse solution were from 0.2 to 0.3 ⁇ m.
  • the coatings of the invention were transparent and slightly iridescent. They were highly uniform and very greatly enhanced the corrosion resistance of the underlying conversion coating based on cerium-rich oxides.

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DE10308237.9A DE10308237B4 (de) 2003-02-25 2003-02-25 Verfahren zur Beschichtung von metallischen Oberflächen, zugehörige Zusammensetzung und ihre Verwendung
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DE10332744.4A DE10332744B4 (de) 2003-07-17 2003-07-17 Verfahren zur Beschichtung von metallischen Oberflächen, Verwendung der nach dem Verfahren beschichteten Substrate und wässerige Zusammensetzung zur Behandlung einer metallischen Oberfläche
DE10332744.4 2003-07-17
PCT/EP2004/001830 WO2004076718A1 (de) 2003-02-25 2004-02-25 Verfahren zur beschichtung von metallischen oberflächen mit einem gemisch enthaltend mindestens zwei silane

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US10/546,583 Abandoned US20060127681A1 (en) 2003-02-25 2004-02-25 Method for coating metallic surfaces with a silane-rich composition
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US12/958,009 Expired - Fee Related US8932679B2 (en) 2003-02-25 2010-12-01 Method for coating metallic surfaces with a mixture containing at least two silanes
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