EP2904131A1 - Procédé de production d'un revêtement sol-gel sur une surface à revêtir d'un composant et composant correspondant - Google Patents

Procédé de production d'un revêtement sol-gel sur une surface à revêtir d'un composant et composant correspondant

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Publication number
EP2904131A1
EP2904131A1 EP12794994.9A EP12794994A EP2904131A1 EP 2904131 A1 EP2904131 A1 EP 2904131A1 EP 12794994 A EP12794994 A EP 12794994A EP 2904131 A1 EP2904131 A1 EP 2904131A1
Authority
EP
European Patent Office
Prior art keywords
voltage
period
anodization
sol
dispersion
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP12794994.9A
Other languages
German (de)
English (en)
Inventor
Hans Binder
Ottmar Binder
Markus KREITMEIER
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.)
Sam Automotive GmbH
Original Assignee
Sueddeutsche Aluminium Manufaktur GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sueddeutsche Aluminium Manufaktur GmbH filed Critical Sueddeutsche Aluminium Manufaktur GmbH
Publication of EP2904131A1 publication Critical patent/EP2904131A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/024—Anodisation under pulsed or modulated current or potential
    • 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
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1212—Zeolites, glasses
    • 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
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/246—Chemical after-treatment for sealing layers

Definitions

  • the invention relates to a method for producing a sol-gel coating on a surface to be coated of an aluminum or aluminum alloy component, comprising the steps of: anodizing the surface by applying an electrical voltage for a given anodizing period to form an anodization layer on the surface; and forming the sol-gel coating on the surface.
  • the invention further relates to a component made of aluminum or an aluminum alloy.
  • Both the anodization and the application of a sol-gel coating on the surface of a component consisting of aluminum or an aluminum alloy for protecting the surface against environmental influences are basically known from the prior art. By means of both procedures can be achieved, in particular against oxidation insensitive, but still easy to clean and visually handsome surface.
  • the layer adhesion of the sol-gel coating is based on the one hand by a chemical and on the other hand by a mechanical bond.
  • the mechanical connection is influenced by the structure or topography of the anodized surface.
  • the corrosion resistance of the surface should be further increased.
  • the voltage applied for anodizing is increased continuously at the beginning of the anodization period with a certain voltage gradient in the direction of a holding voltage maintained over the remainder of the anodization period, in particular to the holding voltage.
  • the voltage gradient is at most 0.5 V / s.
  • the material present in the region of the surface is selectively oxidized or converted in such a way that an oxidic layer is present.
  • Anodization therefore forms an anodization layer on the surface, in particular an oxide layer, which protects deeper layers of the component from corrosion.
  • the anodization layer may also be referred to as a protective layer.
  • the component is at least partially, but in particular completely immersed in a bath of an electrolyte. Subsequently, an electrical voltage is applied to the component over the determined anodization period, the component preferably being used as the anode and an electrode arranged in the bath container accommodating the electrolyte being used as the cathode.
  • the bath container itself or at least a portion of the bath container can be used as a cathode.
  • Anodizing may also be referred to as anodizing.
  • the electrical voltage is now set to the holding voltage at the beginning of the anodization period, so that there is a sudden jump in voltage or the voltage is applied to the holding chip at least within a very short period of time. is set.
  • the applied voltage is preferably increased continuously in the direction of the holding voltage, in particular starting from a voltage of 0V at the beginning of Anodisierzeitraums. This is particularly preferably carried out with the specific voltage gradient, which is constant, for example.
  • the voltage gradient is finite in particular at any time, so there is no voltage jump as in known from the prior art method. It can either be provided to initially only increase the voltage in the direction of the holding voltage or to increase it to the holding voltage with the specific voltage gradient.
  • the voltage gradient is, for example, at most 20V / s, at most 10V / s, at most 7.5V / s, at most 5V / s, at most 3V / s or at most 2V / s, but preferably at most 1V / s, at most 0.5V / s, at most 0.25V / s, at most 0.1V / s, at most 0.075V / s, at most 0.05V / s, at most 0.025V / s or at most 0.01V / s.
  • the holding voltage is that voltage which is maintained over the remainder of the anodizing period.
  • This remainder of the anodizing period has a duration of more than zero seconds.
  • the remainder of the anodization period - which may also be referred to as a voltage hold period - is at least as long as the period from the beginning of the anodization period to a first time reaching the hold voltage.
  • the latter period can also be referred to as a build-up period.
  • the anodization period is composed of a total of two areas, namely the voltage buildup period and the voltage hold period.
  • the duration of the voltage holding period is a multiple of the duration of the voltage build-up period, that is, for example, at least twice, at least three times, at least four times or at least five times as long.
  • the voltage gradient is averaged over the voltage build-up period, for example. It does not have to be constant over the buildup period. However, this is exactly what can be provided. However, as already explained, the voltage gradient is preferably finite at all times; the course of the electrical voltage over time so steadily.
  • the voltage applied for the anodization is preferably understood to mean a setpoint voltage which is set on an anodization device used for anodizing.
  • An actually present actual voltage can now either correspond to the nominal voltage or run after it with a time delay.
  • the actual voltage constantly corresponds to the target voltage; However, it may at least slightly differ from this at times.
  • the applied voltage can also be considered as the actual actual voltage.
  • the voltage is set, whereupon the current intensity adjusts accordingly. The current runs after the voltage so in this case.
  • Changing, in particular increasing the voltage at the beginning of the anodizing period may be referred to as "ramping up" of the voltage
  • This ramping up is performed during the voltage build-up period after which the holding voltage is reached and then maintained during the voltage hold period a duration of at least one second, at least two seconds, at least three seconds, at least four seconds, at least five seconds, at least 7.5 seconds, or at least 10 seconds, but preferably at least 15 seconds, at least 30 seconds, at least 45 seconds, at least 60 seconds, at least 120 seconds, at least 180 seconds, at least 240 seconds, at least 300 seconds, at least 450 seconds, or at least 600 seconds.
  • the lower the electrical voltage applied to anodize the surface the smaller are the cells formed at the beginning of the anodization period. Consequently, at lower voltage, more cells per unit area of the surface and, correspondingly, a larger number of pores are formed. This increased number of pores favors the mechanical bonding of the sol-gel coating to the anodized surface.
  • the current density can be selected as a parameter. Also, according to an alternative embodiment of the method, this can also be increased in the direction of a holding current density or up to the holding current density during the specific period of time which has a certain length.
  • forming the sol-gel coating on the surface comprises the steps of: applying a dispersion to the surface, wherein a coating material is colloidally dispersed in the dispersion; Drying the dispersion to form a gel film on the surface; and curing the gel film to form the sol-gel coating.
  • the dispersion is applied to the surface, for example, immediately after the anodization.
  • a Be Anlagenungsmatenal is present as a colloid.
  • the coating material is formed for example by hydrolysis and condensation of at least one precursor or a precursor compound of the dispersion.
  • the hydrolysis and the condensation take place partly concurrently and competitively.
  • the coating material may also be added to prepare the dispersion.
  • the dispersion can be prepared as a colloidal solution.
  • this is preferably not only the coating material, in particular in the form of particles, but also a particle network at least partially crosslinking polymer network.
  • This polymer network is formed, for example, by silanes.
  • Alcoholates of metals or non-metals can be used as precursors for the dispersion.
  • a silicon precursor is used, for example tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS) or tetraisopropyl orthosilicate (TPOT).
  • TMOS tetramethyl orthosilicate
  • TEOS tetraethyl orthosilicate
  • TPOT tetraisopropyl orthosilicate
  • alkoxides of other metals, transition metals or non-metals for example alkoxides of aluminum or titanium.
  • a solvent for example, ethanol and / or water.
  • a catalyst in particular an acidic or basic catalyst may be provided.
  • the acidic catalyst used is, for example, hydrogen chloride or hydrochloric acid. Additionally or alternatively, nitric acid, acetic acid or sulfuric acid or a mixture of said acids can be used.
  • the basic catalyst used is, for example, sodium hydroxide or sodium hydroxide solution.
  • the hydrolysis can, for example, by the reaction equation
  • M is a metal or semimetal, for example silicon.
  • the dispersion is in the form of a sol.
  • a sol ethanol is used as solvent
  • a hydrosol water is used as solvent
  • the coating material which is subsequently colloidal that is to say in the form of colloids, is formed by the reactions taking place, in particular therefore the hydrolysis and the condensation.
  • the dispersion After the dispersion has been applied, it is dried so that a gel film, in particular xerogel film, forms on the surface. Drying is to be understood as meaning at least partial, in particular complete, application or removal of the solvent used from the dispersion.
  • drying may already result from the application because the layer thickness of the dispersion is usually low, at least when the viscosity of the dispersion is low, compared with the extent or surface area. Accordingly, the solvent can evaporate quickly even under normal ambient conditions.
  • the drying of the dispersion is initiated, for example, immediately after the application of the dispersion or results automatically.
  • the gel film is formed on the surface or the anodization layer, in which there is a loose network of the coating material.
  • the network can not yet be fully linked and have a correspondingly high porosity of, for example, at least 50%. This means in particular that in at least part of the particles of the coating material there is no bond, for example via oxygen, to a further particle.
  • the gel film can be cured to finally form the sol-gel coating.
  • This curing is usually carried out at a high temperature of at least 100 ° C, at least 1 10 ° C, at least 120 ° C, at least 130 ° C, at least 140 ° C, at least 150 ° C, at least 200 ° C, at least 250 ° C, at least 300 ° C, at least 350 ° C or at least 400 ° C.
  • the gel film is preferably converted into a solid ceramic layer with low porosity, namely in the sol-gel coating.
  • the temperatures mentioned are hereby preferably indicated as the so-called “peak metal temperature” (PMT), which occurs during the curing in the component, ie as the component maximum temperature.
  • PMT peak metal temperature
  • the resulting layer thickness of the sol-gel coating is, for example, 0.5 ⁇ m to 10 ⁇ m, in particular 1 ⁇ m to 5 ⁇ m, particularly preferably 1 ⁇ m to 2 ⁇ m.
  • the layer thickness is at least 1 ⁇ , at least 2 ⁇ , at least 5 ⁇ or at least 10 ⁇ .
  • the dispersion is applied correspondingly with a layer thickness with which the desired resulting layer thickness is achieved. Drying and curing are also carried out with parameters with which the desired layer thickness of the sol-gel coating can be achieved. Particularly preferably, the curing of the gel film takes place immediately after the drying of the dispersion, in which the gel film is formed.
  • the voltage is increased in the successive periods at the beginning of the Anodisierzeitraums with certain voltage gradients to the holding voltage, wherein the voltage gradients are different for immediately consecutive periods of time.
  • the said periods of time are parts of the build-up period which begins at the beginning of the anodization period and continues until the first time the holding voltage is reached by the applied voltage.
  • the holding voltage is thus not reached during a single period during which the voltage is continuously increased. Rather, several such periods are provided, in each of which the voltage is increased with a respective, particular voltage gradient.
  • the voltage gradient is preferably finite and, moreover, can be constant at least during the respective period, but alternatively can also be variable.
  • the voltage gradient is to be understood, in particular in the latter case, for example as a mean voltage gradient during the respective period. Nevertheless, the voltage gradient is preferably finite at any time within the respective period, so that the course of the voltage over time is continuous. At the beginning of the first period, which is at the beginning of the anodization period, the voltage is zero. At the end of the last of the consecutive periods, it corresponds to the holding voltage. Additionally or alternatively, however, at least one period of constant or even declining voltage may also be provided.
  • the periods preferably follow one another directly.
  • the voltage gradient here too is, for example, at most 20 V / s, at most 10 V / s, at most 7.5 V / s, at most 5 V / s, at most 3 V / s or at most 2 V / s, but preferably at most 1 V / s, at most 0.5 V / s, at most 0.25V / s, at most 0.1V / s, at most 0.075V / s, at most 0.05V / s, at most 0.025V / s or at most 0.01V / s.
  • the voltage gradient is selected smaller in a first of the time periods than in an immediately following second one of the time periods. This is the case in particular when the voltage gradient of the respective one of the two periods is constant. As already explained above, it can be achieved by means of a lower or lower voltage present at the beginning of the anodization period that the cells or pores formed by the anodization have smaller dimensions than with a larger voltage. If, for example, the first of the time periods, which has the smaller voltage gradient, is located at the beginning of the anodization period, then a large number of pores are formed on the surface because the voltage rises only slowly.
  • the number of pores is no longer reduced, but only the rate of growth of the anodization layer formed by the anodization is increased. It may be provided that the voltage is increased to the holding voltage only in the first and second of the periods, so that no further periods are provided and in the second of the periods the voltage reaches the holding voltage.
  • the anodization layer is compacted after the anodization and before the dispersion is applied at a specific compression temperature, in particular only partially compressed.
  • a specific compression temperature in particular only partially compressed.
  • the dispersion immediately after the anodization on the surface or the anodization is applied.
  • the compression or partial compression is carried out in order to at least partially close the pores, at least on a side facing an environment of the component, or to reduce the dimensions of their opening facing the environment.
  • the compacting is carried out, for example, as hot compacting in demineralized water or as cold compacting.
  • the anodization layer After densification, active hydroxyl groups are present on the anodization layer, which are produced by compaction and promote chemical bonding of the sol-gel coating, in particular silanes contained in it. For this reason, the compression is always beneficial. However, if the anodization layer is completely densified, drying of the dispersion or hardening of the gel film can lead to the formation of layer cracks in the anodization layer. These reduce the advantageous visual impression of the component provided with the sol-gel coating. For this reason, the anodization layer is preferably only partially compressed.
  • a total compression period is determined according to which experience shows that complete compaction is present, and for partial compaction compression is only over a part of the total compaction period, in particular at most 90%, at most 75% maximum 50%, maximum 25% or maximum 10%. It is particularly advantageous to compress only over at most 5%, at most 4%, at most 3%, at most 2%, at most 1%, at most 0.5%, not more than 0.25%, not more than 0.1%, not more than 0.05% or not more than 0.01% of the total compaction period.
  • the overall compaction period is usually chosen to be longer, the greater the layer thickness of the anodization layer. It designates the period of time after which a certain proportion of the pores are completely compressed for the first time, ie closed to an environment.
  • the proportion is for example at least 90%, at least 95%, at least 99% or 100%.
  • the duration n of the total compression period may be considered
  • the component or at least the anodization layer is treated only over the specified part of the total compression period, ie in the case of hot compression, for example by immersion in demineralized water, which has a temperature greater than 60 ° C.
  • the coating material particles in particular polymer particles, for example silicon dioxide particles having a particle size of at most 30 nm, in particular at most 20 nm, preferably at most 10 nm, particularly preferably at most 6 nm or 4nm at the most.
  • the particles are formed, for example, as explained above, by the reactions taking place in the dispersion or in the sol, namely the hydrolysis and the condensation. If a silicon alkoxide is used as the precursor, the particles are present as polysilicate particles, in particular silicon dioxide particles. Additionally or alternatively, the particles can of course be added to produce the dispersion, in particular additionally added.
  • the particle size is defined, for example, as an extent in the direction of the greatest extent of the particles or alternatively as a particle diameter in the case of round or spherical particles.
  • the particle size may alternatively be understood as mean particle diameter.
  • all particles of the coating material ie all particles contained in the dispersion, have the stated particle sizes. Alternatively, however, this may also be provided for only a part of the coating material, so that particles with the specified particle size can be used. However, for example, larger particles may be present.
  • the particle size is understood as mean particle size or mean particle diameter of all particles contained in the dispersion. This average particle size should meet the conditions mentioned.
  • the particles are limited in size by the values given above, for example, they have a particle size of at least 2 nm, preferably at least 4 nm. In a particularly preferred embodiment, all particles of the coating material have particle sizes between 4 nm and 6 nm.
  • the dispersion is prepared by mixing a plurality of starting dispersions with particles having different particle sizes. Depending on the precursor and the concentration, different particle sizes are established in different dispersions. These dispersions are referred to as starting dispersions.
  • the dispersion used to prepare the sol-gel coating should now be prepared by mixing several of these starting dispersions. be prepared so that in the dispersion particles with different particle sizes.
  • both “small” and “large” particles may be present in the dispersion, with the “small” particles having, for example, particle sizes of 2 nm to 10 nm, preferably from 4 nm to 6 nm, and the “large” particle particle sizes of 10nm to 30nm, for example from 15nm to 20nm.
  • the starting dispersions are mixed together to form the dispersion in a certain mixing ratio.
  • provision may be made for the voltage gradient, in particular the voltage gradient at the beginning of the anodization period, to be determined as a function of the particle size, the voltage gradient being selected smaller for smaller particle sizes. It has already been stated above that the pores formed by the anodization have smaller dimensions at lower voltages than at larger voltages.
  • the dispersion is a fluorosilane and / or a Fluorsilanzurung with a certain volume fraction, preferably at most 10% by volume, at most 7.5% by volume, at most 5% by volume, at most 4% by volume, at most 3 vol -%, not more than 2% by volume, not more than 1% by volume or not more than 0,5% by volume, is added as an additive. Also higher volume fractions, for example of at most 25% by volume, at most 20% by volume, at most 15% by volume, may be provided. Fluorine-containing substances are hydrophobic.
  • the fluorosilane preparation or a fluorosilane after curing is applied to the sol-gel coating in the form of a topcoat in order to achieve this property.
  • this is disadvantageous because the fluorosilane or the preparation is removed over time from the surface, for example by abrasion, and may also be harmful to health under certain circumstances.
  • These disadvantages are avoided by incorporating the fluorosilane or fluorosilane preparation in the dispersion.
  • the fluorosilane or the preparation is added directly to the dispersion, so that it is present directly after curing in the sol-gel coating. Also in this way the hydrophobic effect can be achieved.
  • the disadvantage is that the fluorosilane or the preparation may adversely affect the bonding of the sol-gel coating to the surface. This is also due to its hydrophobic
  • experiments have surprisingly shown that the use of particles having a small particle size as described above can reduce this negative effect of the fluorosilane or of the preparation.
  • the particles displace the fluorosilane or the preparation of the anodized surface, so that it is no longer present in an adjacent to the anodization layer boundary layer of the sol-gel coating below. Rather, it is shifted in the direction of the environment.
  • This also causes a very advantageous increase in the concentration of the fluorosilane or the preparation on the side facing the environment of the sol-gel coating, whereby the hydrophobic effect is still improved there.
  • the addition of the fluorosilane or the preparation thus provides a very easy-to-clean surface, without having to accept disadvantages in the connection of the sol-gel coating to the surface. This is the case in particular when small particle sizes according to the above statements, in particular particle sizes of at most 10 nm, at most 8 nm, at most 6 nm or at most 4 nm are used.
  • the fluorosilane preparation may be a fluoroalkyl silane,
  • a fluoroalkyl-functional silane in particular 3,3,4,4,5,5,6,6,7, 7,8,8,8-tridecafluorooctyltriethoxysilane containing. This is available, for example, from Evonik under the name "Dynasylan® F 8261.”
  • the fluorosilane preparation may contain at least one solvent, for example isopropanol and / or water.
  • the invention also relates to a component made of aluminum or an aluminum alloy, in particular a motor vehicle component, having a sol-gel coating applied to a surface of the component, produced by the method according to the preceding statements.
  • a component made of aluminum or an aluminum alloy in particular a motor vehicle component, having a sol-gel coating applied to a surface of the component, produced by the method according to the preceding statements.
  • the advantages of the process have already been discussed.
  • the component and the method can be developed according to the above statements, so that reference is made to this extent.
  • the invention relates, for example, to a component made of aluminum or an aluminum alloy, in particular a motor vehicle component, with a sol-gel coating applied to a surface of the component, preferably produced by the method according to the preceding embodiments, wherein an anodization layer formed by anodization is formed on the surface is present with a pore structure and the anodization is carried out by applying an electrical voltage over a certain Anodisierzeitraum to form the anodization at the surface.
  • the component is present, for example, as a motor vehicle component, in particular as an outboard motor vehicle component.
  • the component may represent a decorative automotive component.
  • the sol-gel coating is particularly preferably outboard, so is subjected to environmental conditions.
  • the pore structure is formed by continuously increasing the voltage applied for anodization at the beginning of the anodization period with a certain voltage gradient in the direction of a holding voltage maintained over the remainder of the anodization period, in particular to the holding voltage.
  • the voltage gradient is, for example, at most 0.5 V / s, although the above-mentioned voltage gradients can also be used.
  • the component is preferably produced by means of the method explained. The component and the method can be developed according to the above statements, so that reference is made to this extent.
  • the special implementation of the anodization results in a pore structure which has a very high pore density. It is suitably well suited to achieve an excellent bonding of the sol-gel coating.
  • the invention relates to a device for producing a sol-gel coating on a surface to be coated of a component made of aluminum or an aluminum alloy, in particular for carrying out the method according to the preceding embodiments, wherein the device is designed to carry out the following steps: Anodizing the surface by applying an electrical voltage for a given anodization period to form an anodization layer on the surface; and forming the sol-gel coating on the surface.
  • the device is furthermore designed to continuously adjust the voltage applied for anodization at the beginning of the a-nodalizing period with a specific voltage. gradient in the direction of a maintained over the remainder of the Anodisierzeitraums holding voltage, in particular to increase the holding voltage.
  • the voltage gradient is, for example, at most 0.5 V / s or selected according to the above statements.
  • the device described above is preferably designed for carrying out the method according to the invention.
  • the above statements, in particular the embodiments relating to the method can be used analogously for the device, which can be designed or developed accordingly for implementation.
  • each possible embodiment of the method can be assigned a corresponding configuration of the device.
  • Figures 1 to 7 are diagrams in which in each case the course of the voltage applied for anodizing voltage over time for various embodiments of the inventive method is plotted.
  • a profile of a voltage U over time t is plotted for at least part of an anodization period.
  • the voltage U is applied to anodize a surface of a member made of aluminum or an aluminum alloy during an anodization period of duration At E to form an anodization layer on the surface.
  • it is now planned to release the voltage continuously increase with a certain voltage gradient in the direction of a holding voltage UH ZU maintained over a remainder of the Anodisierzeitraums with the duration At H , in particular to increase to this.
  • the current flow is interrupted, ie the voltage U is set equal to zero.
  • the period from the beginning of the anodizing period, in which the voltage is preferably equal to zero, until the first reaching of the holding voltage U H may be referred to as a voltage build-up period.
  • This is composed of the successive periods with the durations At-i, At 2 and so on.
  • the buildup period is immediately followed by the remainder of the anodization period, which may also be referred to as the voltage hold period.
  • the duration of the voltage hold period is at least equal to or more than the duration of the buildup period.
  • the voltage hold period is at least twice, three times, four times, or five times as long as the build up period. In the exemplary embodiment illustrated in FIG.
  • the voltage build-up period only extends over the single period of duration At-i, during which the voltage is continuously increased with a constant voltage gradient up to the holding voltage UH. Subsequently, the voltage is constant over the voltage holding period.
  • two time periods are provided, namely with the durations At- 1 and At 2 , which form the voltage build-up period together.
  • the voltage build-up period is followed by the voltage build-up period.
  • the first period is shorter than the second period (Ati ⁇ At 2 ), while for the embodiments of Figures 4, 5 and 7 is reversed (At-i> At 2 ).
  • the voltage gradient in the first period is greater than in the second period. This is in turn reversed in the embodiments of Figures 4, 5 and 7.
  • the voltage build-up period extends in all embodiments, for example over a period of at least 15 seconds, at least 30 seconds, at least 45 seconds, at least 60 seconds, at least 120 seconds, at least 180 seconds, at least 240 seconds or (as shown in the figures) at least 300 seconds , However, it lasts at most 1200 seconds, at most 900 seconds, at most 600 seconds or at most 450 seconds.
  • the holding voltage is for example 10 volts to 20 volts, in particular 15 volts.
  • the anodization of the surface is preferably followed by partial compression of the anodization layer produced by the anodization at.
  • This partial compression takes place over a specific compression period, which forms part of a total compression period.
  • This total compaction period is determined as a function of the layer thickness of the anodization layer on the basis of suitable relationships.
  • the total compression period describes the period over which compression must be carried out in order to completely densify the anodization layer, ie the time until which time a majority, ie at least 90%, at least 95% or at least 99% of the pores of the Anodization completely closed for the first time against an environment of the component.
  • the partial compression takes place over a compression period of 30 seconds at a temperature of a fluid used for compression, for example demineralized water, of 70 ° C.
  • a fluid used for compression for example demineralized water
  • the compression times are 30 seconds, 80 seconds, 60 seconds, 180 seconds, 60 seconds and 200 seconds, respectively, while the temperatures are 65 ° C, 70 ° C, 98 ° C, 95 ° C, 90 ° ° C or 80 ° C.
  • a dispersion is applied to the surface or the anodization layer present thereon.
  • a coating material is colloidally dispersed, with particles, in particular silicon dioxide particles, having a specific particle size being used as the coating material.
  • the preferred particle size is for the embodiments of Figures 1 to 3, 6 and 7 10nm to 20nm and for the embodiments of Figures 4 and 5 4nm to 6nm.
  • the dispersion is subsequently applied to the application to Forming a gel film dried and cured the gel film to produce the sol-gel coating.

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Abstract

L'invention concerne un procédé de production d'un revêtement sol-gel sur une surface à revêtir d'un composant en aluminium ou en alliage d'aluminium, comportant les étapes suivantes : anodisation de la surface par application d'une tension électrique pendant un intervalle d'anodisation défini pour créer une couche d'anodisation sur la surface ; et création du revêtement sol-gel sur la surface. Selon l'invention, au début de l'intervalle d'anodisation, la tension appliquée pour l'anodisation est augmentée en continu avec un gradient de tension défini en direction d'une tension de maintien conservée au cours du reste de l'intervalle d'anodisation, notamment jusqu'à atteinte de la tension de maintien. L'invention concerne également un composant en aluminium ou en alliage d'aluminium.
EP12794994.9A 2012-10-08 2012-12-05 Procédé de production d'un revêtement sol-gel sur une surface à revêtir d'un composant et composant correspondant Withdrawn EP2904131A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE201210019969 DE102012019969A1 (de) 2012-10-08 2012-10-08 Verfahren zum Herstellen einer Sol-Gel-Beschichtung auf einer zu beschichtenden Oberfläche eines Bauteils sowie entsprechendes Bauteil
PCT/EP2012/074457 WO2014056552A1 (fr) 2012-10-08 2012-12-05 Procédé de production d'un revêtement sol-gel sur une surface à revêtir d'un composant et composant correspondant

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EP2904131A1 true EP2904131A1 (fr) 2015-08-12

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US11939490B2 (en) 2017-07-31 2024-03-26 Momentive Performance Materials Inc. Curable surface-protective coating composition, processes for its preparation and application to a metallic substrate and resulting coated metallic substrate

Citations (3)

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EP0802267A1 (fr) * 1996-04-18 1997-10-22 Alusuisse Technology & Management AG Surfaces d'aluminium avec des couleurs d'interférence
US5693208A (en) * 1995-03-16 1997-12-02 Alusuisse Technology & Management Ltd. Process for continuously anodizing strips or wires of aluminum
EP1486588A2 (fr) * 2002-10-10 2004-12-15 Süddeutsche Aluminium Manufaktur GmbH Procédé pour hydrater l'oxyde de métal posé sur des pièces en métal, aussi bien que les pièces hydratées

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DE10361888B3 (de) * 2003-12-23 2005-09-22 Airbus Deutschland Gmbh Anodisierverfahren für Aluminiumwerkstoffe
FR2886309B1 (fr) * 2005-05-31 2007-08-17 Airbus France Sas Sol pour le revetement par voie sol-gel d'une surface et procede de revetement par voie sol-gel le mettant en oeuvre
EP1835002B1 (fr) * 2006-03-14 2014-07-23 Cerasol Hong Kong Limited Composition de revêtement céramique non collante et procédé
EP1884578A1 (fr) * 2006-07-31 2008-02-06 MPG Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Méthode de fabrication d'une structure poreuse d'oxide d'aluminium auto-organisée, article nanoporeux, et nano-objet.
DE102008011296A1 (de) * 2007-03-16 2008-09-18 Süddeutsche Aluminium Manufaktur GmbH Kraftfahrzeug-Bauteil mit Sol-Gel-Beschichtung
US20080274375A1 (en) * 2007-05-04 2008-11-06 Duracouche International Limited Anodizing Aluminum and Alloys Thereof
US7732068B2 (en) * 2007-08-28 2010-06-08 Alcoa Inc. Corrosion resistant aluminum alloy substrates and methods of producing the same
WO2012029570A1 (fr) * 2010-08-30 2012-03-08 シャープ株式会社 Procédés de formation de couche anodisée et de fabrication de moule

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Publication number Priority date Publication date Assignee Title
US5693208A (en) * 1995-03-16 1997-12-02 Alusuisse Technology & Management Ltd. Process for continuously anodizing strips or wires of aluminum
EP0802267A1 (fr) * 1996-04-18 1997-10-22 Alusuisse Technology & Management AG Surfaces d'aluminium avec des couleurs d'interférence
EP1486588A2 (fr) * 2002-10-10 2004-12-15 Süddeutsche Aluminium Manufaktur GmbH Procédé pour hydrater l'oxyde de métal posé sur des pièces en métal, aussi bien que les pièces hydratées

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Title
See also references of WO2014056552A1 *

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WO2014056552A1 (fr) 2014-04-17

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