US20140011020A1 - Promoting the adhesion of a surface of a titanium material - Google Patents

Promoting the adhesion of a surface of a titanium material Download PDF

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Publication number
US20140011020A1
US20140011020A1 US13/993,928 US201113993928A US2014011020A1 US 20140011020 A1 US20140011020 A1 US 20140011020A1 US 201113993928 A US201113993928 A US 201113993928A US 2014011020 A1 US2014011020 A1 US 2014011020A1
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range
titanium
adhesion
titanium material
promoting layer
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US13/993,928
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Tobias Mertens
Martin Beneke
Franz J. Gammel
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Airbus Operations GmbH
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Airbus Operations GmbH
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Assigned to AIRBUS OPERATIONS GMBH reassignment AIRBUS OPERATIONS GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BENEKE, MARTIN, GAMMEL, FRANZ J., MERTENS, TOBIAS
Publication of US20140011020A1 publication Critical patent/US20140011020A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
    • 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
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/10—Presence of inorganic materials
    • C09J2400/16—Metal
    • C09J2400/163—Metal in the substrate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/10—Presence of inorganic materials
    • C09J2400/16—Metal
    • C09J2400/166—Metal in the pretreated surface to be joined
    • 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
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256—Heavy metal or aluminum or compound thereof

Definitions

  • the invention relates to a method for promoting the adhesion of a surface of a titanium material and to a vehicle, in particular an aircraft, comprising a titanium material having a surface and an organic material that is associated with the surface with good adhesion.
  • Promoting the adhesion of a surface of a titanium material is known.
  • the adhesion of organic materials such as adhesive, paint, sealant and/or the like to titanium materials is determined by the condition of the surface of the titanium material.
  • the adhesion of the surface of the titanium material can be promoted beforehand, which in the simplest case consists of a cleaning step. It is also known, optionally after the cleaning step, to carry out a physical and/or chemical treatment of the surface of the titanium material, wherein wettability, chemical compatibility and/or mechanical anchoring of the organic material can be influenced.
  • Known processes include mechanical roughening, for example by way of radiation, chemical etching and a formation of adhesive layers by way of chemical and/or electrochemical conversion, for example phosphating and/or anodizing and/or applying coatings.
  • U.S. Pat. No. 4,473,446 discloses a method for treating the surfaces of titanium parts prior to bonding by way of anodizing in a chromic-hydrofluoric acid bath at an anodizing voltage between one volt and 5 volts.
  • U.S. Pat. No. 4,394,224 discloses a method for treating titanium parts or titanium alloy parts so as to create an adhesion-promoting oxide layer.
  • the document includes the steps of applying to and treating the surface with a mixture of aqueous solutions made of sodium hydroxide and hydrogen peroxide, maintaining the applied mixture within a temperature range in which the hydrogen peroxide is relatively stable, and causing an increased rate of oxidation at the surface region.
  • DE 34 27 543 A1 relates to an alkaline bath for treating titanium.
  • the bath is made of an alkali hydroxide, a titanium complexing agent, and a foreign ion complexing agent.
  • U.S. Pat. No. 3,907,609 discloses a chemical conversion process and a composition for producing an adherent conversion coating on titanium and titanium alloys.
  • 6,037,060 relate to a surface treatment, preferably for titanium and aluminum alloys, for forming a sol gel film covalently bonded on a metal surface to produce strong and durable adhesive bonds between the metal and an organic adhesive without using toxic chemicals and while significantly reducing and/or eliminating rinse water requirements of conventional anodizing and/or etching processes.
  • DE 38 02 043 C1 relates to a method for preparing a metal surface.
  • a layer is applied to a metal surface by way of sand blasting using a substance that is composed of 0.1 to 30% by weight optionally silanized, amorphous silicon-containing material having a grain size of less than 1 ⁇ m, the remainder being a sand blasting substance having a mean grain size of greater than 1 ⁇ m, and this layer subsequently being optionally silanized.
  • DE 10 2006 045 951 A1 relates to a method for chemically modifying and/or activating solid surfaces.
  • halogen-containing compounds are supplied by simultaneously adding organosilicon compounds or silanes or organometallic compounds or silicon hydrides or metal hydrides to the carrier material.
  • WO 2009/015329 A2 relates to a method for forming a perpendicularly oriented titanium nanotube field using electrochemical oxidation.
  • WO 2006/104644 A2 relates to a surface-modified implant, comprising at least one metal-containing surface, comprising a plurality of nanotubes on the surface, wherein the nanotubes have an oxide of the metal-containing surface.
  • 7,695,767 B2 relates to a method for providing a superhydrophobic surface on a structure, for example airfoils, propellers and/or rotors.
  • the method includes applying a hydrofluoric acid-containing medium to a titanium substrate.
  • US 2010 0028387 A1 relates to a titanium or titanium alloy substrate, coated with a molecular plasma made of deposited polypeptides, wherein the substrate has a nanotubular-structured surface.
  • WO 2009/017945 A2 relates to nanotubularly structured titanium substrates coated with nano-particulate hydroxylapatite (nano-HA).
  • the object is achieved by a method for promoting the adhesion of a surface of a titanium material.
  • the method includes creating an adhesion promoting layer that is fixed to the surface of the titanium material and comprises nanotubes, which include titanium dioxide and have diameters of 10 to 300 nm, in particular 20 to 220 nm, in particular 30 to 180 nm, in particular 40 to 140 nm, in particular 50 to 100 nm, on the surface, and applying an organic material to the adhesion promoting layer comprising the nanotubes with good adhesion. It was found that the combination of the nanotubes having the indicated dimensioning with the organic material allows for particularly long-term stable and high-strength joining of the organic material to the titanium material.
  • the surface can be understood to mean a surface of the titanium material, in particular before applying the adhesion promoting layer.
  • the surface of the titanium material is coated with the organic material.
  • delamination of the organic material from the titanium material can be reliably prevented.
  • the coating is achieved by way of the adhesion promoting layer, which for this purpose is located between and/or in a boundary region between the surface and the organic material.
  • a further material is bonded to the surface comprising the nanotubes by way of an adhesive layer of the organic material.
  • a long-term stable and high-strength bond is obtained between the titanium material and the further material.
  • structural bonding of a component comprising the titanium material to a further component by way of a bond comprising the adhesive layer of the organic material is provided for.
  • structural bonds, in particular for creating a supporting structure, between the titanium material, or the component made of the titanium material, and the further component can be implemented.
  • a bond can be understood to mean in particular an adhesive surface, an adhesive point and/or a plurality of adhesive points.
  • anodic oxidation of the surface of the titanium material so as to generate the nanotubes of the adhesion promoting layer is provided for.
  • the adhesion promoting layer can advantageously be produced in an environmentally friendly manner by way of anodic oxidation.
  • the titanium material comprises an alloy Ti6Al4V, wherein anodic oxidation of the surface takes place in an electrolyte having a composition of 50 to 250 g/l, in particular 120 to 140 g/l, preferably 130 g/l ammonium sulfate, and 0.5 to 10 g/l, in particular 4 to 6 g/l, preferably 5 g/l ammonium fluoride, at a temperature of 10 to 60° C., in particular 20 to 30° C., preferably 25° C., and a voltage of preferably 2 to 50 volts, in particular 10 to 20 volts for 5 to 480 minutes, in particular 20 to 40 minutes, preferably 30 minutes.
  • anodic oxidation of the surface takes place in an electrolyte having a composition of 50 to 250 g/l, in particular 120 to 140 g/l, preferably 130 g/l ammonium sulfate, and 0.5 to 10 g/l, in particular 4 to 6 g/l, preferably
  • the indicated electrolytes advantageously have re-dissolution properties, wherein the nanotubes can advantageously be produced in the desired dimension using the indicated parameters. It is possible to create a layer thickness of 100 to 750 nm and a pore diameter of approximately 15 to 80 nm.
  • a vehicle in particular an aircraft, comprising a titanium material having a surface and an organic material that is associated with the surface with good adhesion.
  • an adhesion promoting layer is disposed between the surface and the organic material, the layer being fixed to the surface of the titanium material, associated with the organic material with good adhesion and comprises nanotubes include contain titanium dioxide and have diameters of 10 to 300 nm, in particular 20 to 220 nm, in particular 30 to 180 nm, in particular 40 to 140 nm, preferably 50 to 100 nm.
  • Advantageously long-term stable and high-strength joining of the organic material to the titanium material by way of the adhesion promoting layer is achieved.
  • the vehicle comprises a component comprising the titanium material and the adhesion promoting layer, the component being structurally bonded to a further component of the vehicle by way of an adhesive layer of the organic material.
  • a supporting structure of the vehicle can be created using the structural bond, the structure satisfying the requirements in terms of corrosion resistance and/or stability.
  • the adhesion promoting layer has a thickness of 100 nm to 10 ⁇ m, in particular 200 nm to 1 ⁇ m, in particular 250 to 800 nm, in particular 280 to 600 nm, in particular 300 to 500 nm.
  • a long-term stable adhesion promoting layer can be implemented in the indicated thicknesses.
  • FIG. 1 is a partially illustrated aircraft comprising a structural bond of a component with a titanium material and a further component;
  • FIG. 2 is a side view of an electron microscopy image of an anodization layer
  • FIG. 3 is a top view onto the anodization layer shown in FIG. 2 ;
  • FIG. 4 is a top view onto a joining point between a component comprising a titanium material and a further component after a butt-joint test;
  • FIG. 5 is a comparison chart of an aging test by way of a wedge test using three different adhesion promoting methods.
  • FIG. 1 is a partial view of an aircraft 1 comprising a component 3 , which comprises and/or consists of a titanium material 5 .
  • a titanium material can be understood to mean titanium and/or a titanium alloy.
  • the component 3 is structurally bonded to a further component 7 by way of an adhesive layer 9 , in particular a glued layer of an adhesive.
  • the further component 7 can comprise any arbitrary material, in particular an aluminum material, a fiber-reinforced plastic material or likewise a titanium material.
  • the adhesive layer 9 is fixed to the component 3 by way of an adhesion promoting layer 11 .
  • the adhesion promoting layer 11 comprises nanotubes 13 , which comprise titanium dioxide.
  • the component 3 can be a metal sheet made of the alloy Ti6Al4V, for example. This is immersed in an electrolyte composed of 130 g/l ammonium sulfate and 5 g/l ammonium fluoride. The electrolyte is advantageously free of hydrofluoric acid.
  • anodization is carried out at a temperature of 25° C. using a voltage of 10 to 20 volts for 30 minutes.
  • a regularly structured, porous oxide layer having a thickness of approximately 400 to 500 nm is created.
  • the upper open pores, which advantageously form the nanotubes 13 have pore diameters of approximately 40 to 80 nm.
  • FIG. 2 shows a corresponding result.
  • FIG. 2 shows an electron microscopy image of the adhesion promoting layer 11 in a so-called cryo fracture, wherein the adhesion promoting layer 11 comprises and/or consists of the nanotubes 13 , so-called TiO 2 nanotubes, which is to say the anodization layer.
  • FIG. 3 shows a top view onto the adhesion promoting layer 11 , which is shown in FIG. 2 , of the anodization layer on the titanium material 5 Ti6Al4V.
  • Adhesion was tested by way of a butt-joint test according to ISO 4624.
  • a Ti6Al4V metal sheet which is to say the component 3 , for example, was pretreated by way of the previously described method and bonded to a chromic acid-anodized aluminum plunger, for example the further component 7 .
  • An epoxy adhesive a two-component construction adhesive, known by the brand name Scotch-Weld® DP 490, available from 3M, was used as the glue for the adhesive layer 9 .
  • This adhesive has a tensile shear resistance of 26 MPa (at 23° C. and with pickled aluminum).
  • purely cohesive failure in the adhesive which is to say in the adhesive layer 9 , was found in the tested samples, which is shown in greater detail in FIG. 4 .
  • FIG. 5 shows a graph 15 , wherein a time between 0 and 1000 h is plotted on an x-axis 17 and a crack length between 20 mm and 100 mm is plotted on a y-axis 19 .
  • a total of three crack curves which is to say a first crack curve 21 for alkaline pickling, a second crack curve 23 for the previously described method according to the invention, and a third crack curve 25 for the NaTESi method are plotted. It is apparent that the previously described method according to the invention achieves the values of the NaTESi method and is consequently equivalent to the same.
  • Long-term stable nanostructured titanium surfaces can advantageously be created by way of the previously described method in a particularly environmentally friendly manner, which provide a suitable substrate for long-term stable and/or high-strength organic coatings. It is conceivable to apply only a coating, instead of the adhesive layer 9 , to the adhesion promoting layer 11 .
  • the method according to the invention advantageously results in long-term stable nanostructured titanium surfaces.
  • This structuring which is to say the plurality of nanotubes 13 , makes structural bonds exhibiting long-term stability possible, in particular in aircraft construction, which advantageously makes new design concepts possible (see FIG. 1 ).
  • delamination of paints, in particular on titanium rivets can advantageously be reliably prevented by way of the pre-treatment, wherein advantageously the costs for re-painting can be avoided and optionally maintenance intervals can be saved.
  • the adhesion promoting layer 11 can be created on the component 3 comprising the titanium material 5 , wherein this layer can advantageously be provided with coatings that have good adhesion and are made of organic materials such as adhesive, paint, sealant and the like, wherein high adhesion and long-term stability of the corresponding coatings and/or bonds are achieved.
  • the basis of the method is the creation of a stable oxide layer on the titanium surface of the titanium material 5 by way of anodic oxidation in an electrolyte, wherein this electrolyte advantageously comprises constituents that are not harmful to the environment.
  • electrolytes are used for the titanium pre-treatment, by way of which porous surface morphologies can be produced on titanium in a targeted manner. All electrolytes that exhibit re-dissolution properties and are therefore suitable for creating pore structures are suited, wherein the diameters thereof range between 10 and 300 nm, 20 and 220 nm, in particular 30 and 180 nm, in particular 40 to 140 nm, preferably 50 to 100 nm.
  • Suitable thicknesses of the oxide layers which is to say of the adhesion promoting layer 11 , range between 100 nm and 10 ⁇ m, in particular 200 nm and 1 ⁇ m, in particular 250 and 800 nm, in particular 280 and 600 nm, preferably 300 to 500 nm.
  • the method according to the invention advantageously does not comprise or use any hydrofluoric acid, which is to say is free of hydrofluoric acid, wherein advantageously a lower potential for risk exists.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
US13/993,928 2010-12-14 2011-12-12 Promoting the adhesion of a surface of a titanium material Abandoned US20140011020A1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
DE102010054473.6 2010-12-14
DE102010054473 2010-12-14
DE102011112117.3 2011-09-02
DE102011112117A DE102011112117A1 (de) 2010-12-14 2011-09-02 Haftvermitteln einer Fläche eines Titanwerkstoffs
PCT/DE2011/002105 WO2012079563A2 (de) 2010-12-14 2011-12-12 Haftvermitteln einer fläche eines titanwerkstoffs

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EP (1) EP2652058B1 (de)
CN (1) CN103261347B (de)
DE (1) DE102011112117A1 (de)
WO (1) WO2012079563A2 (de)

Cited By (11)

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US20130177738A1 (en) * 2010-10-21 2013-07-11 Peter Mardilovich Method of forming a micro-structure
US20150299889A1 (en) * 2011-12-22 2015-10-22 Eads Deutschland Gmbh Self-Cleaning and Superhydrophobic Surfaces Based on TIO2 Nanotubes
JP2015190039A (ja) * 2014-03-28 2015-11-02 国立大学法人岩手大学 多孔質陽極酸化皮膜の製造方法及び多孔質陽極酸化皮膜
US20170042682A1 (en) * 2015-08-11 2017-02-16 Biomet 3I, Llc Surface treatment for an implant surface
JP2017510717A (ja) * 2014-03-14 2017-04-13 エアバス・ディフェンス・アンド・スペース・ゲーエムベーハー 水および氷をはじく特性を有する磨かれたナノ構造金属表面の製造方法ならびに使用
EP3243651A4 (de) * 2014-12-25 2018-08-08 BYD Company Limited Metallharzverbundstoff und herstellungsverfahren dafür sowie gehäuse für elektronisches produkt
US10287697B2 (en) 2010-10-21 2019-05-14 Hewlett-Packard Development Company, L.P. Nano-structure and method of making the same
US10426577B2 (en) 2015-08-11 2019-10-01 Biomet 3I, Llc Surface treatment for an implant surface
US20200383223A1 (en) * 2019-05-28 2020-12-03 Apple Inc. Titanium surfaces with improved color consistency and resistance to color change
US10927472B2 (en) 2010-10-21 2021-02-23 Hewlett-Packard Development Company, L.P. Method of forming a micro-structure
USRE49451E1 (en) 2015-10-15 2023-03-07 Samsung Electronics Co., Ltd. Electronic device case and material layer details of the same

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10287697B2 (en) 2010-10-21 2019-05-14 Hewlett-Packard Development Company, L.P. Nano-structure and method of making the same
US10927472B2 (en) 2010-10-21 2021-02-23 Hewlett-Packard Development Company, L.P. Method of forming a micro-structure
US9751755B2 (en) * 2010-10-21 2017-09-05 Hewlett-Packard Development Company, L.P. Method of forming a micro-structure
US20130177738A1 (en) * 2010-10-21 2013-07-11 Peter Mardilovich Method of forming a micro-structure
US20150299889A1 (en) * 2011-12-22 2015-10-22 Eads Deutschland Gmbh Self-Cleaning and Superhydrophobic Surfaces Based on TIO2 Nanotubes
JP2017510717A (ja) * 2014-03-14 2017-04-13 エアバス・ディフェンス・アンド・スペース・ゲーエムベーハー 水および氷をはじく特性を有する磨かれたナノ構造金属表面の製造方法ならびに使用
JP2015190039A (ja) * 2014-03-28 2015-11-02 国立大学法人岩手大学 多孔質陽極酸化皮膜の製造方法及び多孔質陽極酸化皮膜
EP3243651A4 (de) * 2014-12-25 2018-08-08 BYD Company Limited Metallharzverbundstoff und herstellungsverfahren dafür sowie gehäuse für elektronisches produkt
US10022232B2 (en) * 2015-08-11 2018-07-17 Biomet 3I, Llc Surface treatment for an implant surface
US10426577B2 (en) 2015-08-11 2019-10-01 Biomet 3I, Llc Surface treatment for an implant surface
US20170042682A1 (en) * 2015-08-11 2017-02-16 Biomet 3I, Llc Surface treatment for an implant surface
US11918433B2 (en) 2015-08-11 2024-03-05 Biomet 3I, Llc Surface treatment for an implant surface
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