EP4330035A1 - Structure composite polymère ayant une couche d'ancrage en polymère d'aluminium, et procédé d'attaque - Google Patents

Structure composite polymère ayant une couche d'ancrage en polymère d'aluminium, et procédé d'attaque

Info

Publication number
EP4330035A1
EP4330035A1 EP22711472.5A EP22711472A EP4330035A1 EP 4330035 A1 EP4330035 A1 EP 4330035A1 EP 22711472 A EP22711472 A EP 22711472A EP 4330035 A1 EP4330035 A1 EP 4330035A1
Authority
EP
European Patent Office
Prior art keywords
aluminum
polymer
steel
partial structure
etching
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.)
Pending
Application number
EP22711472.5A
Other languages
German (de)
English (en)
Inventor
Mark-Daniel GERNGROSS
Melike Baytekin-Gerngroß
Jürgen CARSTENSEN
Rainer Adelung
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.)
Christian Albrechts Universitaet Kiel
Original Assignee
Christian Albrechts Universitaet Kiel
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 Christian Albrechts Universitaet Kiel filed Critical Christian Albrechts Universitaet Kiel
Publication of EP4330035A1 publication Critical patent/EP4330035A1/fr
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/012—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of aluminium or an aluminium alloy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
    • B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
    • B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
    • B32B3/30—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by a layer formed with recesses or projections, e.g. hollows, grooves, protuberances, ribs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B7/04—Interconnection of layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/08—Interconnection of layers by mechanical means
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/04—Etching of light metals
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/03—3 layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/732—Dimensional properties
    • B32B2307/737—Dimensions, e.g. volume or area
    • B32B2307/7375—Linear, e.g. length, distance or width
    • B32B2307/7376—Thickness
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12556—Organic component
    • 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
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    • Y10T428/12556—Organic component
    • Y10T428/12569—Synthetic resin
    • 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
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    • Y10T428/12736—Al-base component
    • Y10T428/1275—Next to Group VIII or IB metal-base component
    • Y10T428/12757—Fe
    • 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
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    • Y10T428/12979—Containing more than 10% nonferrous elements [e.g., high alloy, stainless]
    • 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
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    • 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
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    • 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
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Definitions

  • the invention relates generally to a steel-polymer composite structure comprising an aluminum-polymer anchoring layer and a method for etching the surface of aluminum-coated metals, and/or, in particular, aluminized steels.
  • the invention relates to a steel-polymer composite structure having an aluminum-polymer anchoring layer, the composite structure
  • a layered structure consisting of a first, second and third partial structure running at least in one direction from the middle of the first partial structure is formed, so that the first partial structure made of steel is at least partially covered and/or connected to the second partial structure made of aluminum or an aluminum alloy, wherein the second partial structure is at least partially covered and/or connected to the third partial structure.
  • the invention also relates to an etching method for anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys in a workpiece coating made of aluminum or aluminum alloys or in a surface made of aluminum or aluminum alloys of a workpiece or a steel-polymer composite structure having an aluminum-polymer anchoring layer.
  • adhesion to steels is increased by mechanical methods such as grit blasting, milling and the like, which methods produce an increase in the surface area of the substrate.
  • chemical etching processes to increase the surface area, which allow the steel surface to oxidize even more easily, which ultimately leads to the well-known disadvantages of oxides. In any case, such etching processes do not lead to an undercut structure in the steels discussed here.
  • Another way to improve it is to coat the steel surfaces with layers of metal.
  • Metals that are susceptible to corrosion, in particular iron and structural steel are usually coated with a rapidly oxidizing and thus chemically passivating protective layer made of aluminum or an aluminum alloy. Such a protective layer can, for example, be deposited galvanically on the metals. For metals with high melting temperatures, immersion in molten aluminum is also usually a quicker and cheaper method of producing a coating.
  • a silicon-containing aluminum alloy with, for example or typically 8-11% silicon by mass is usually used as the coating.
  • Common coating thicknesses for construction steel are around 80 - 150 g/m2, i.e. the coatings are usually a few 10 microns thick.
  • FIGS. 6a and b images of the surface of pure aluminum after an etching attack with hydrochloric acid can be seen in FIGS. 6a and b shown there. 1 in the publication US 2013/0264196 A1, which does not deal with the mechanical anchoring, but with the surface enlargement of aluminum anodes in electrolytic capacitors, and therefore particularly deep pores electrochemically etches. These pores would penetrate the applied Al layer and destroy the corrosion protection of the Al layer. In addition, hydrogen embrittlement of the underlying steel substrate can occur there.
  • the document DE 102016 113641 A1 discloses a heterostructure comprising at least a first partial surface containing copper alone and at least a second partial surface opposite the first partial surface containing aluminum alone or an aluminum alloy, wherein a. an anchoring layer arranged between the first and second partial surface, wherein b. each interface perpendicular to the anchoring layer has at least one island of aluminum or aluminum alloy surrounded by copper and c. at most the previously known mixed crystals of the aluminum alloy occur in the anchoring layer. Furthermore, the invention relates to an aluminum-copper connector and a heterostructure production method.
  • publication DE 2320099 A shows a method for producing a plastic substrate with a roughened surface by laminating an aluminum foil with a rough surface onto a plastic substrate with heating and pressure and subsequent chemical etching of the aluminum foil.
  • the invention relates to a process for the production of plastic substrates with surfaces roughened in such a way that they are able to firmly anchor thin, electrolessly applied metal layers or layers applied as inks, Indian ink or paints.
  • Hydrogen embrittlement is an additional negative effect.
  • Hydrogen embrittlement is a glaring disadvantage, especially in the case of steel-polymer composites that are subjected to high mechanical loads, as it reduces the mechanical properties of the steel to such an extent that they fail or can lead to cracks/fractures even under low static or dynamic mechanical loads.
  • hydrogen embrittlement is bad for the reliability of such steel-polymer composites, since the composite can also fail close to the surface within the steel component.
  • the aim of the invention disclosed here is that steel-polymer composites are improved. These composites have a very wide range of applications and can range from simple two-layer systems to multi-layer systems to, for example, wire mesh composites or coated individual wires/strips.
  • the aluminum layer applied to the steel substrate which is known in the prior art, functions, as already explained, as corrosion protection for the steel substrate. After the surface has been treated according to the invention, ie in particular after a nanoscale sculpting process, this layer should or can also function as a mechanical adhesion promoter via “mechanical interlocking”.
  • the object of the invention can also be seen as enabling the production of steel-polymer composites in which there is no adhesive failure between steel and polymer due to the undercut structures in the Al/Al alloy surface firmly adhering to the steel surface.
  • An essential secondary condition here is that no hydrogen embrittlement should occur and no closed oxide layers should be produced.
  • the problem or problems are solved with a steel-polymer composite structure according to the main claim and can be further solved by an etching method according to the independent claim.
  • the steel-polymer composite structure has an aluminum-polymer anchoring layer, with the composite structure
  • a layered structure consisting of a first, second and third partial structure running at least in one direction from the middle of the first partial structure is formed, so that the first partial structure made of steel is at least partially covered and/or connected to the second partial structure made of aluminum or an aluminum alloy, wherein the second partial structure is at least partially covered with the third partial structure and/or is connected, and is characterized in that
  • the thickness of the first partial structure is greater than and/or equal to that of the second partial structure
  • an anchoring layer connects the second and third partial structure directly to one another, the anchoring layer having anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys, which flowed around and/or were surrounded by material of the third partial structure that was still in the liquid state during manufacture and/or or are filled, and
  • the thickness of the anchoring layer can be in particular between 0.5 and 100 micrometers or particularly preferably between 10 and 50 micrometers. This represents a further relevant feature of the invention that is also preferred, since the anchoring layer according to the invention, the thickness of which is in particular between 10 and 50 micrometers, or even in the range from 0.5 to 100 micrometers, has significantly higher maximum roughness.
  • the anchoring layer connects the second and the third partial structure to one another, the anchoring layer having anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys, which flowed around and/or surrounded and/or were surrounded by the material of the third partial structure that was still in the liquid state during production. or filled.
  • the flowed and/or enclosed and/or filled islands and/or undercuts have a cuboid and/or nested cuboid shape, a minimum size of 200 nanometers and sharp and/or rounded edges.
  • a preferred design variant of the steel-polymer composite structure is the following combination of features:
  • the steel-polymer composite structure has an aluminum-polymer anchoring layer, with the composite structure
  • first substructure consisting solely of steel
  • second partial structure consisting solely of aluminum or an aluminum alloy and adjoining at least partial areas of the first partial structure and applied there and
  • a layered structure consisting of a first, second and third partial structure running at least in one direction from the middle of the first partial structure is formed, so that the first partial structure made of steel is at least partially covered and/or connected to the second partial structure made of aluminum or an aluminum alloy, wherein the second partial structure is at least partially covered and/or connected to the third partial structure, and is characterized in that
  • the thickness of the first partial structure is greater than and/or equal to that of the second partial structure
  • an anchoring layer connects the second and third partial structure directly to one another, the anchoring layer having anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys, which flowed around and/or were surrounded by material of the third partial structure that was still in the liquid state during manufacture and/or or are filled,
  • the thickness of the anchoring layer is between 10 and 50 microns
  • the steel-polymer composite structure can be designed such that
  • any cut surface running perpendicular to the anchoring layer in the area of the anchoring structure at least one island made of polymer or polymer fiber composite surrounded by aluminum or aluminum alloy, or Having polymer particle composite, and / or
  • any cut surface running perpendicularly to the anchoring layer in the region of the anchoring structure has at least one island made of aluminum or aluminum alloy surrounded by polymer or polymer fiber composite or polymer particle composite.
  • the previously known mixed crystals including the intermetallic phases of the aluminum alloy, can occur in the anchoring layer.
  • the etching method according to the invention can be used for anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys in a workpiece coating made of aluminum or aluminum alloys or in a surface made of aluminum or aluminum alloys of a workpiece or a steel - Polymer composite structure having an aluminum-polymer anchoring layer, characterized in that the etching takes place:
  • an aqueous electrolyte solution with a low chlorine ion concentration of less than 0.8 mmol/cm 3 the electrolyte being provided in particular as an aqueous solution of a chlorine salt;
  • the electrolyte can be provided as an aqueous solution of a chlorine salt, in particular one of the salts sodium chloride or potassium chloride or calcium chloride being provided to provide the chlorine ion concentration.
  • the workpiece can be formed from a corroding metal, in particular steel, and the coating or surface is an anti-corrosion layer, with the corroding metal, ie the steel, not being etched.
  • the method disclosed here can be carried out much more cheaply and faster, since strongly oxidizing acids can be dispensed with.
  • the object according to the invention differs in a special way from the prior art, in particular in that undercut structures are created on the surface-structured aluminum surface or aluminum alloy surface by electrochemical structuring, which are then replaced by a flowable polymer (hardening thermally, hardening at RT or solidifying [thermoplastic]) are enclosed.
  • the high-strength steel-aluminum polymer composite itself or the electrochemical structuring process for the Al/Al alloy surface firmly adhering to the steel surface can be produced with the formation of undercut structures, i.e. in particular cuboid structures, without hydrogen embrittlement occurs in the steel component or a build-up of thick oxide layers (such as those that occur during anodizing, for example).
  • the method claimed here differs from the prior art in particular in the etching current density and the etching duration.
  • the average etching current density is larger than 1 A/cm 2 .
  • etching is performed at an etching current density in the range from 10 mA/cm 2 to 100 mA/cm 2 , so that the etching current densities used in the prior art are one to two powers of ten below the etching current density used in the present method according to the invention. lie.
  • the etching time according to the this-side etching method is less than 60 seconds. In the exemplary embodiments listed in the prior art, the etching time is 30 minutes, among other things. In addition, it is also explicitly shown in the prior art that etching takes place uniformly and slowly everywhere. Therefore, the etch durations disclosed in the prior art are thus completely contrary to the etch duration of the etch process on this side.
  • the electrolyte is formed as an aqueous solution of a chlorine salt.
  • Electrolyte according to the prior art is provided, for example, as a mixture of several salts, for example as an aqueous solution of sodium chloride and sodium sulfate.
  • etching is carried out at an etching current density in the interval from 10 mA/cm 2 to 100 mA/cm 2 (cf. the acknowledged prior art in the introduction).
  • diffusion limitation of the passivation species sets in.
  • the publication US 2013/0264196 A1 states that etching takes place at an etching current density of 100 to 1000 mA/cm 2 and diffusion limitation of the passivation species occurs. Therefore, from the prior art, high etching current densities with aqueous electrolytes on the order of magnitude of the etching process disclosed on this page are not suggested or suggested.
  • a slow etch is in stark contrast to the less than 60 second etch time of this inventive method.
  • Etching times on the order of magnitude of the method on this side cannot regularly be used with known methods of the prior art, since otherwise the desired results in relation to the heterostructure cannot be achieved with the specified method parameters.
  • the fact that the person skilled in the art of electrochemistry is familiar with the fact that he has to adapt the etching time to the new circumstances when an etching parameter is changed does not apply here either.
  • the contrast between uniformly slow etching with a duration of 30 minutes, for example, and an etching process of less than 60 seconds is also so great that this no longer represents an adjustment within the “normal framework”, but a new process.
  • the electrolyte is provided as an aqueous solution of a chlorine salt.
  • it can contain at least one of the salts sodium chloride, potassium chloride or calcium chloride.
  • the electrolyte for the direct electrolytic etching is preferably provided as an aqueous alkali solution such as sodium carbonate or sodium hydroxide solution, or as an aqueous acid such as hydrochloric acid.
  • This etching process according to the invention has an aqueous electrolyte with a low chlorine ion concentration of less than 0.8 mmol/cm, whereas the aqueous electrolyte containing chlorine ions according to the prior art is 0.5 to 5% by weight Sodium chloride solution is provided.
  • an alkaline or acidic electrolytic solution is in complete contrast to the use of a chlorine salt according to the present invention.
  • the electrolyte according to this method is environmentally friendly, easy to dispose of, easy to handle and easy to produce.
  • An acid or base as an electrolyte, as is used in the prior art, is subject to certain safety regulations that must be observed.
  • no anchoring structures with undercuts and/or enclosed islands made of aluminum or aluminum alloys are regularly created in a workpiece coating made of aluminum or aluminum alloys or in a surface made of aluminum or aluminum alloys of a workpiece or a steel-polymer composite structure, the surrounded and/or surrounded and/or filled islands and/or undercuts have a cuboid and/or nested cuboid shape and a minimum size of 200 nanometers and sharp and/or rounded edges, as would be possible according to the method of this invention. There are just no undercuts with a cuboid and/or nested cuboid shape.
  • the possible uses of the composite according to the invention can be seen in particular in a wide variety of areas, such as e.g. aviation, the automotive industry, architecture (sheet metal parts coated with paint, inserts in fiber composite materials to increase strength), medical technology (orthopedic components coated with e.g. silicone), etc.
  • the following configuration can preferably be used in terms of process technology to design structured steel with an Al alloy layer as a component by etching accordingly with a structure, namely in that:
  • the electrochemical cell is coated with steel with an Al alloy layer as the anode, the Al layer being in contact with the electrolyte;
  • the power source can be used with a wide current density range, for example 1A/cm 2 for 15s, with the following general rule: higher current densities lead to shorter process times with the same electrolyte concentration
  • the electrolyte temperature can typically be room temperature, although higher/lower temperatures are also possible;
  • an electrolyte with 0.2 mol/l NaCl in water can be run in order to achieve the desired etching results
  • the CI concentration can also be provided via HCl or other chlorides
  • the aluminized steel surfaces can be structured in particular by electrochemical etching. Using this process, aluminized steel surfaces can be structured regardless of the layer thickness of the highly aluminum-rich coating. In one embodiment, the structuring can take place in a simple electrochemical cell consisting of a counter-electrode and the aluminized steel surface as the working electrode. Overall, very short etching times are preferable in order not to dissolve too much of the aluminum layer, since this also serves as an anti-corrosion layer on the steel. At least one interface between structured steel with an Al alloy layer and polymer in various geometric shapes, such as flat multilayers, wires, wire mesh, strips, spheres, etc. can be produced in this way.
  • various composites can be produced, also with different polymers at the same time, e.g. layer sequence polymer1 - steel with aluminum alloy layer - polymer2.
  • Coating can be done, for example, by dipping/spraying in a polymer that is initially free-flowing and then hardens, e.g. duroplastics and elastomers, but also thermoplastics. Resin transfer molding of composite materials with structured steel with Al alloy layer inserts is also possible. In addition, methods of thermal spraying known in the prior art, including injection molding, powder coating, painting and the like are also possible.
  • the steel structure has a suitable and undamaged corrosion protection through the aluminum or Al alloy layer, which leads to a very high corrosion resistance;
  • Fig. 1 shows a composite consisting of a steel-aluminum-coating-alloy component structured on one side and a polymer, with a first surface being designed accordingly here. An interface is formed between the polymer and the structured steel-aluminum alloy component.
  • the general layered structure of the first partial structure made of steel, followed by the second partial structure made of aluminum or an aluminum alloy and the third partial structure made of the polymer material can be seen here, with the second and third partial structure together forming a common anchoring structure.
  • Fig. 2 shows a composite consisting of a structured steel-aluminum alloy component and polymer, with a first and a second side or even surrounding the entire structure being designed accordingly.
  • a multi-layer system is formed here, with the steel-aluminum alloy component being able to have any shape, for example plate, wire, sphere, meshwork and the like.
  • Fig. 3 shows a nanoscale sculptured hot-dip aluminized steel in a plan view.
  • Fig. 3a shows a typical section of the aluminized steel surface after structuring. It can be seen that the surface has been completely structured. Here, differently structured areas are already recognizable, which are shown in Fig. 3b) at a higher magnification.
  • Figure 3c) is an exemplary representation of one of the millions of these partially free-standing barb structures composed of cuboids on the structured surface.
  • these cuboid structures are always oriented at right angles to one another. Individual areas can - as can be seen in Fig. 3c) in the upper right area - are rotated relative to each other, depending on the crystallographic orientation of the near-surface grains. These cuboid structures not only occur very close to the surface, but also occur in depth, as shown in the left part of Fig. 3c). In addition to the cuboid structures, Fig. 3c) also shows parts of the dendritic structures - see upper left and lower right area. These structures show a very smooth surface without the formation of a microstructure worth mentioning. An enlargement of the cuboid structures can be seen in Fig. 3d).
  • the typical sizes of the cuboids are in the range of a few tens of nanometers for the finest structures down to the low micrometer range.
  • the partially free-standing cuboid structures form a mechanical interlocking structure.
  • Fig. 4 shows an EDX of nanoscale sculptured hot-dip aluminized steel in a plan view.
  • the element distribution of the structured aluminized steel surface examined by EDX is shown.
  • the cuboid structures described in Fig. 3 are made of aluminum, while the dendrite structures are silicon precipitates.
  • the iron signal also shows a spatial dependence in the element distribution and is more pronounced at the points where the Si-rich dendrite structures are preferentially located.
  • traces of oxygen are found on the structured surface both in the more Al-rich and in the more Si-rich areas on the surface. These are due to the formation of the native oxide layer on the aluminum and silicon structures.
  • Fig. 5 shows a plan view of a fracture surface of a nanoscale sculptured hot-dip aluminized steel-epoxy composite.
  • Fig. 6 shows a plan view of a fracture surface (top left) and EDX of a nanoscale sculptured hot-dip aluminized steel-epoxy composite.
  • the element distribution of the structured aluminized steel surface examined by EDX is shown.

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Abstract

La présente invention concerne une structure composite acier-polymère ayant une couche d'ancrage en polymère d'aluminium, la structure composite étant constituée - d'une première sous-structure qui est constituée uniquement d'acier, - d'une deuxième sous-structure qui est constituée uniquement d'aluminium ou d'un alliage d'aluminium et qui est adjacente à au moins des sous-régions de la première sous-structure et est appliquée sur celle-ci, et - d'une troisième sous-structure qui est constituée uniquement d'un polymère, de composite fibre-polymère, ou de composite de particules de polymère et qui est adjacente à au moins des sous-régions de la deuxième sous-structure et est appliquée sur celle-ci, une structure de couche qui s'étend à partir du centre de la première sous-structure au moins dans une direction étant constituée de la première, de la deuxième, et de la troisième sous-structure de telle sorte que la première sous-structure en acier est au moins partiellement recouverte par et/ou est raccordée à la deuxième sous-structure en aluminium ou en alliage d'aluminium, et la deuxième sous-structure est au moins partiellement recouverte par et/ou est raccordée à la troisième sous-structure. La présente invention concerne en outre un procédé d'attaque de structures d'ancrage.
EP22711472.5A 2021-04-29 2022-03-13 Structure composite polymère ayant une couche d'ancrage en polymère d'aluminium, et procédé d'attaque Pending EP4330035A1 (fr)

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DE102021111149.8A DE102021111149A1 (de) 2021-04-29 2021-04-29 Polymer-kompositstruktur aufweisend eine aluminium-polymer verankerungsschicht sowie ätzverfahren
PCT/DE2022/100201 WO2022228601A1 (fr) 2021-04-29 2022-03-13 Structure composite polymère ayant une couche d'ancrage en polymère d'aluminium, et procédé d'attaque

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DE102024111115A1 (de) 2024-04-19 2025-10-23 Christian-Albrechts-Universität zu Kiel, Körperschaft des öffentlichen Rechts Gepulstes anodisches ätz-herstellungsverfahren von verzahnungsstrukturen auf oberflächen von kupfer und/oder kupferlegierungen, kupfer und/oder kupferlegierungen
DE102024122239A1 (de) * 2024-08-05 2026-02-05 Ulman Dichtungstechnik Gmbh Verbundmembran sowie Verfahren zur Herstellung

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US2944917A (en) 1954-12-13 1960-07-12 Marc Gregoire Method of coating a metal base with polytetrafluoroethylene
JPS5123266B2 (fr) 1972-04-21 1976-07-15
JPS54158480A (en) 1978-06-05 1979-12-14 Sumitomo Electric Ind Ltd Resin-coated article
CA1154637A (fr) * 1980-07-26 1983-10-04 Fumio Matsuyama Methode pour former une membrure d'acier plaquee d'aluminium et enduite de resine et membrure ainsi formee
JP3924593B1 (ja) * 2006-05-25 2007-06-06 ラミネート工業株式会社 ラミネート金属板の製造方法と該方法により製造されたラミネート金属板
US8535507B1 (en) 2008-01-11 2013-09-17 Pacesetter, Inc. Electrochemical drilling system and process for improving electrical porosity of etched anode foil
US20110111214A1 (en) * 2008-06-12 2011-05-12 Masanori Endo Integrally injection-molded aluminum/resin article and process for producing the same
DE102016102379B3 (de) * 2016-02-11 2016-11-03 Christian-Albrechts-Universität Zu Kiel Verfahren zur Ätzung der Oberfläche von Aluminium-Kleinkörpern, Aluminium-Kleinkörper mit geätzter Oberfläche und solche Kleinkörper enthaltende Materialverbunde
DE102016113641A1 (de) 2016-07-25 2018-01-25 Christian-Albrechts-Universität Zu Kiel Aluminium-Kupfer-Konnektor aufweisend eine Heterostruktur und Verfahren zur Herstellung der Heterostruktur

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