EP3332050A1 - Revêtement sol-gel adhérent et résistant à l'abrasion appliqué sur l'aluminium et procédé de production d'un tel revêtement - Google Patents

Revêtement sol-gel adhérent et résistant à l'abrasion appliqué sur l'aluminium et procédé de production d'un tel revêtement

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Publication number
EP3332050A1
EP3332050A1 EP16745479.2A EP16745479A EP3332050A1 EP 3332050 A1 EP3332050 A1 EP 3332050A1 EP 16745479 A EP16745479 A EP 16745479A EP 3332050 A1 EP3332050 A1 EP 3332050A1
Authority
EP
European Patent Office
Prior art keywords
sol
gel
coating
aluminum
gel coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP16745479.2A
Other languages
German (de)
English (en)
Other versions
EP3332050B1 (fr
Inventor
Siegfried Piesslinger-Schweiger
Olaf Boehme
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.)
Sepies GmbH
Original Assignee
Sepies GmbH
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Filing date
Publication date
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Publication of EP3332050A1 publication Critical patent/EP3332050A1/fr
Application granted granted Critical
Publication of EP3332050B1 publication Critical patent/EP3332050B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48—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
    • C23C22/56—Treatment of aluminium 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/04—Pretreatment of the material to be coated
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
    • 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
    • C23C22/82—After-treatment
    • C23C22/83—Chemical 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1283—Control of temperature, e.g. gradual temperature increase, modulation of temperature

Definitions

  • the present invention relates to an abrasion-resistant and adherent sol-gel coating on aluminum surfaces and to a process for its production. Moreover, the present invention relates to a process for the surface treatment of aluminum in order to improve the adhesion of subsequently applied sol-gel coatings.
  • Sol-gel layers impart high corrosion resistance and temperature resistance to metal surfaces. In addition, they improve the cleaning ability and protect the surfaces from fingerprints and dirt. Therefore, sol-gel coatings offer significant economic and qualitative advantages.
  • Sol-gel coatings on surfaces of stainless steel, steel, copper and copper alloys generally have a sufficiently high adhesive strength that allows deformation of coated surfaces, for example, by bending or edges without peeling of the coating and prevents detachment by rubbing or wiping.
  • sol-gel coatings on surfaces of aluminum and aluminum alloys have a significantly lower adhesive strength.
  • Sol-gel coatings applied directly to aluminum surfaces without special pretreatment of the surfaces are obtained by bending, even with slight deformation of the surfaces big bending radii, cracked and come off. They can be partially rubbed off with a thumb or fingernail.
  • the low adhesive strength is due to the properties of the natural oxide layers, which are formed by the influence of oxygen from the environment, and protect the aluminum from corrosion.
  • WO 01/59179 A1 discloses a process for the surface treatment of, inter alia, aluminum in a two-stage chemical process associated with mechanical abrasion. Initially, the surface is treated with sulfuric acid such that a fresh, i. oxide-free, metal surface is produced. That is, following the treatment of the surface with an acid, fresh oxide layers are formed on the metal in an oxidative process.
  • US 5,356,492 A describes a non-toxic process for the treatment of aluminum surfaces, in which the corrosion resistance can be improved by subsequent treatment with an alkaline solution containing molybdate, nitrite and metasilicate ions.
  • the layer thus obtained can then be further improved in terms of its corrosion resistance by applying a sol-gel layer.
  • treatment with, for example, hydrogen peroxide in a multi-step process can improve the adhesion of the sol-gel coating to the aluminum surface, especially if the sol-gel coating is applied immediately after treatment with the oxidizing agent.
  • EP 1 457 267 A1 describes a method for producing formed aluminum sheet metal parts with a decorative surface.
  • the steps are in succession: providing a strip of aluminum, optionally continuous degreasing of the strip, optionally electrochemical, chemical or mechanical glazing of the possibly defatted strip, continuous pretreatment of the possibly degreased and / or shined strip Producing a pretreatment layer suitable as a primer for a lacquer layer.
  • an optional oxide layer on the metal surface is completely removed before the process is carried out (compare page 3, line 14).
  • anodic oxidation of the aluminum is regularly carried out. This process ensures the provision of a porous, anodically produced oxide layer.
  • Aqueous oxidizing agents wherein the aqueous oxidizing agent has a pH in the range of 4 to 8 are used in this
  • US 2004/0177898 A1 describes a method for the treatment of metallic surfaces, such as aluminum surfaces.
  • an oxidizing agent is used together with a sulfate providing agent to obtain a passivated surface, which is to consist essentially of manganese, oxygen, sulfur and carbon.
  • a passivated surface which is to consist essentially of manganese, oxygen, sulfur and carbon.
  • the present invention is based on the finding that aluminum surfaces, which already have a naturally formed oxide layer, can be pretreated with an aqueous, oxidizing solution in such a way that the adhesion of sols Gel coatings on pretreated aluminum surfaces compared to non-pretreated surfaces is significantly improved.
  • the invention relates to a sol-gel-coated aluminum surface obtained by pretreating the surface already provided with an original or naturally formed oxide layer in a first step with an oxidizing aqueous solution, followed by drying and subsequent application and curing of a sol-gel layer.
  • such an oxide layer is understood, which usually forms directly on aluminum surfaces, once their surface has been treated by mechanical or other means so that a bare aluminum layer is obtained.
  • a so-called passive layer is formed, which consists essentially of alumina.
  • Such a natural aluminum oxide layer is regularly insufficient as a primer (see also the examples in the experimental part of this application).
  • abrasion-resistant and adherent sol-gel coatings are obtained on aluminum surfaces, which usually have a layer thickness of 0.5 to 5.0 ⁇ m. These coatings can also be colored. For this purpose, inorganic color pigments are very particularly suitable.
  • aluminum surfaces are used in the present application, they also address aluminum alloys whose chemical behavior is comparable to that of an aluminum surface.
  • the invention particularly relates to a process for the treatment of aluminum surfaces, which are exposed to an aqueous oxidizing solution. Investigations have shown that when treating the oxide layers naturally present on aluminum surfaces with an oxidizing, aqueous medium, these layers are modified such that they are suitable as primer for subsequently applied sol-gel coatings.
  • the aqueous oxidizing agents contain conventional oxidizing agents such as peroxides, persulfates, perchlorates, perborates in an appropriate concentration.
  • oxidizing agents such as potassium persulfate or hydrogen peroxide are also suitable.
  • the aqueous oxidizing agents have a pH in the range of 3 to 8, or 4 to 8.
  • concentration of, for example, hydrogen peroxide is usually in a range of 1 to 30% by weight.
  • Solid oxidizing agents are usually added in an amount of 5 to 50 g / l (for example, 5 to 50 g / l potassium persulfate).
  • the treatment of the surfaces is usually carried out at room temperature by dipping, spraying or wiping for a period of at least 2 minutes, preferably from 5 to 10 minutes.
  • the surfaces are rinsed with water and then dried.
  • the sol-gel coating is applied.
  • Sol-gel coatings are usually obtained from two reaction components, which are mixed shortly before processing in a fixed ratio to each other. This mixture is last added as a third component, a dilution, usually an alcohol. Dilution sets the concentration of the reaction mixture and the viscosity of the final batch.
  • the sol-gel is first applied in the form of a liquid sol having colloidal particles suspended therein, which subsequently converts to a gel and, after thermal curing, finally forms a solid, hard topcoat. So if the "application of the sol-gel coating” or the “thermal curing of the sol-gel coating” is the expert, in which state the sol-gel system is.
  • the sol-gel is preferably a silica sol based on silanes which are dissolved in solvents, wherein the silica sol preferably also contains one or more further sol-forming elements, preferably one or more elements from the group consisting of Al, Ti, Zr, Mg, Ca and Zn, these elements replacing the Si atoms in the colloidal structures.
  • Preferred sol-gel coatings / sol-gel coatings are described in EP2145980. Reference is hereby made in particular to the sol-gel coatings described in EP2145980 and the process for their use.
  • the starting compounds for forming the preferred sols and finally the sol-gel coating are preferably hydrolyzable silanes of the formula SiR 4 , where the 4 radicals R 2-4 comprise hydrolyzable radicals OR 'and 0-2 comprise nonhydrolyzable radicals R "
  • the hydrolyzable radicals OR ' are hydroxy, alkoxy and / or cycloalkoxy radicals. Suitable examples thereof include, for example, hydroxy, methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, i-butoxy, t-butoxy, pentoxy, hexoxy, cyclopentyloxy, cyclohexyloxy, in particular Ethoxy, n-propoxy and isopropoxy are preferred.
  • the hydrolyzable radicals OR ' may be identical or different from one another.
  • the non-hydrolyzable radicals R " are alkyl and / or cycloalkyl radicals, suitable examples of which include, for example, methyl, ethyl, n-propyl, isopropyl, n-butyl, i-butyl, t-butyl, pentyl, hexyl, cyclopentyl, cyclohexyl radicals, particular preference being given to methyl, ethyl, n-propyl and isopropyl radicals
  • the nonhydrolyzable radicals R " may also be identical or different from one another.
  • the starting compounds of the preferred sols can consist of a single type of silane, but often they are mixtures of several silanes (and optionally additional sol-forming starting compounds of other elements).
  • include. It is preferred that at least one of the components of the starting compounds is a silane of the formula Si (OR ') 4-nR "n with n 0, ie Si (OR') 4.
  • a preferred sol-gel lacquer may be the starting materials TEOS
  • MTES ethyltriethoxysilane
  • DMDES dimethyldiethoxysilane
  • the starting compounds are partially hydrolyzed to the corresponding hydroxy compounds (such as orthosilicic acid, trihydroxyalkylsilane, etc.), which may be favored by the addition of a catalyst such as acid. Due to the high tendency for condensation of these hydroxy compounds, these can now condense with elimination of water to form smaller siloxane networks.
  • the sol-gel coating usually has a stoving temperature of less than 300 ° C, preferably from 200 ° C to 250 ° C, on.
  • the sol-gel coating can also be colored, for example by adding inorganic color pigments.
  • degree of coverage with inorganic color pigments i. by the proportion by weight of the inorganic color pigments in the sol-gel, color intensity and depth can be adjusted.
  • the viscosity of the sol-gel varnish can be adjusted by a person skilled in the art. It is known that the sol, with a correspondingly high dilution in its solvent, is sufficiently thin to be sprayed, sprayed, rolled or brushed
  • Suitable solvents for the sol are water and especially alcohols such as methanol, ethanol, n-propanol or isopropanol, with ethanol and isopropanol being preferred because of their physical properties and the low toxicity of their vapors.
  • the sol-gel may include inorganic color pigments, e.g. SICOCER® Black 10901, SICOCER® Blue 2502, or SICOCER® Red 2355 from BASF.
  • inorganic color pigments e.g. SICOCER® Black 10901, SICOCER® Blue 2502, or SICOCER® Red 2355 from BASF.
  • the sol-gel coating is preferably applied by spraying or rolling, spraying or brushing are also possible. Preferably, however, it is done by spraying, since this allows precise control of the amount applied per unit area.
  • the surfaces can be dried until the solvent has evaporated.
  • the dried surfaces are then thermally cured.
  • the thermal curing in step (iii) is preferably carried out at a temperature of less than 300 ° C, preferably in a range of 200 ° C to 300 ° C.
  • the curing takes place for a period of about 20 to 60, preferably 30 minutes at temperatures in the range of 160 ° C to 280 ° C, preferably 200 ° C to 250 ° C in air.
  • the glass-ceramic coating preferably has a thickness of 0.5-5.0 ⁇ m, preferably 1.0-5.0 ⁇ m, or 0.5-3.0 ⁇ m, and most preferably 1.0-3.0 ⁇ m.
  • the glass-ceramic coating preferably has a uniform thickness
  • Variations of preferably less than 10% of the layer thickness are preferably less than 10% of the layer thickness.
  • an aluminum surface with an abrasion-resistant and adherent sol-gel coating is achieved which is distinguished by improved abrasion resistance and adhesion.
  • a particular advantage of the invention lies in the fact that an abrasion-resistant and adherent surface is obtained in a particularly simple, cost-effective and environmentally friendly manner.
  • a further advantage is that, compared to the prior art in the method according to the invention, restrictions with regard to the shape and the size of the workpieces to be treated are hardly to be considered.
  • a sol-gel coating was applied by spraying onto a sheet without further pretreatment and then baked in air at 240 ° C. for a period of 30 minutes. After cooling, the sheet was bent 90 ° by a radius of 10d. The sol-gel layer cracked and broke off in the area of the bend.
  • the second sheet was weighed into a 10% aqueous solution for 10 minutes. Hydrogen peroxide immersed, then rinsed with water and dried. Subsequently, an identical sol-gel coating was applied by spraying and baked at a temperature of 240 ° C for 30 minutes in air. After cooling, the sheet was bent by 180 ° with a radius of 2d. The coating remained free of cracks in the area of the bend, homogeneous and firmly adhering.
  • a sol-gel coating was applied by spraying onto a sheet without further pretreatment and then baked in air at 240 ° C. for a period of 30 minutes. After cooling, the sheet was bent at a radius of 10 d at an angle of 90 °. The sol-gel coating cracked in the area of the bend and came off. The second sheet was weighed for 10 minutes with a 10% aqueous solution. sprayed, then rinsed and dried. Subsequently, an identical sol-gel coating was applied by spraying and baked at a temperature of 240 ° C in air. After cooling, the sheet was bent at a radius of 2d by an angle of 180 °. The coating in the area of the bend remained free of cracks, was homogeneous and firmly adhering.
  • a sol-gel coating was applied by spraying onto a sheet without further pretreatment and then baked in air at 240 ° C. for a period of 30 minutes. After cooling, the sheet was bent at a radius of 10 d at an angle of 90 °. The sol-gel coating cracked in the area of the bend and came off.
  • the second plate was sprayed with an aqueous solution containing 40 g / l potassium persulfate at pH 4 for 5 minutes, then rinsed and dried. Subsequently, an identical sol-gel coating was applied and baked at a temperature of 240 ° C in air. After cooling, the sheet was bent at a radius of 2d by an angle of 180 °. The coating in the area of the bend remained free of cracks, was homogeneous and firmly adhering.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

La présente invention concerne une surface d'aluminium pourvue d'un revêtement sol-gel adhérent et résistant à l'abrasion. Pour obtenir ce revêtement, la surface d'aluminium est traitée par une solution aqueuse oxydante de manière à être appropriée comme fond d'accrochage au revêtement sol-gel consécutif.
EP16745479.2A 2015-08-05 2016-08-02 Revêtement sol-gel résistant à l'usure sur aluminium et procédé de fabrication d'un tel revêtement Active EP3332050B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP15002335 2015-08-05
PCT/EP2016/068377 WO2017021387A1 (fr) 2015-08-05 2016-08-02 Revêtement sol-gel adhérent et résistant à l'abrasion appliqué sur l'aluminium et procédé de production d'un tel revêtement

Publications (2)

Publication Number Publication Date
EP3332050A1 true EP3332050A1 (fr) 2018-06-13
EP3332050B1 EP3332050B1 (fr) 2019-05-08

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EP16745479.2A Active EP3332050B1 (fr) 2015-08-05 2016-08-02 Revêtement sol-gel résistant à l'usure sur aluminium et procédé de fabrication d'un tel revêtement

Country Status (3)

Country Link
US (1) US20180230600A1 (fr)
EP (1) EP3332050B1 (fr)
WO (1) WO2017021387A1 (fr)

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* Cited by examiner, † Cited by third party
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