US20140151235A1 - Process for Producing an Adhesion-Promoting Layer on a Surface of a Titanium Material - Google Patents

Process for Producing an Adhesion-Promoting Layer on a Surface of a Titanium Material Download PDF

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Publication number
US20140151235A1
US20140151235A1 US14/130,817 US201214130817A US2014151235A1 US 20140151235 A1 US20140151235 A1 US 20140151235A1 US 201214130817 A US201214130817 A US 201214130817A US 2014151235 A1 US2014151235 A1 US 2014151235A1
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range
concentration
anodic oxidation
carried out
titanium material
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US14/130,817
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Tobias Mertens
Franz Gammel
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Airbus Defence and Space GmbH
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EADS Deutschland GmbH
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Publication of US20140151235A1 publication Critical patent/US20140151235A1/en
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    • 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

Definitions

  • Exemplary embodiments of the present invention relate to a method for producing an adhesion promoting layer on a surface of a titanium material; an adhesion promoting layer, according to the method, on the surface of a titanium material; as well as the use of an alkaline solution.
  • the production of adhesion promoting layers on a surface of a titanium material is known.
  • the adhesion promoting layer can be used to join organic materials, such as adhesives, paint, sealants and/or the like, to the titanium material.
  • the adhesion promoting layer on the surface of the titanium material can be produced, for example, by means of anodic oxidization; that is, the adhesion promoting layer can consist, for example, of an oxide layer. This oxide layer may be used as the adhesion promoting layer for a subsequent coating of the titanium material with the organic material.
  • U.S. Pat. No. 4,473,446 discloses a method for treating the surface of titanium parts prior to adhesive bonding by anodization in a chromic hydrofluoric acid bath at an anodizing voltage ranging from one volt to 5 volts.
  • U.S. Pat. No. 4,394,224 discloses a method for treating titanium parts or titanium alloy parts in order to generate an adhesion promoting oxide layer. This method includes the steps of: applying to the surface and treating the surface with a mixture of aqueous solutions comprising 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 on the surface area.
  • German patent document DE 34 27 543 A1 relates to an alkaline bath for the treatment of titanium.
  • the bath is composed of an alkali hydroxide, a titanium complexing agent, and an impurity 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.
  • 5,814,137 and 6,037,060 relate to a surface treatment, preferably for titanium and aluminum alloys, in order to form a sol gel film, which adheres to the metal surface by means of covalent bonds, in order to generate a strong and durable adhesive bond between the metal and an organic adhesive without using toxic chemicals and while at the same time significantly reducing and/or eliminating the rinse water requirements of conventional anodizing and/or etching processes.
  • German patent document DE 38 02 043 C1 relates to a method for preparing a metal surface.
  • a layer is applied to a metal surface by sandblasting with a material consisting of 0.1 to 30% by weight of an optionally silanized, amorphous silicon containing material having a grain size of less than 1 ⁇ m, and the rest of the material is a sandblasting medium having a mean grain size of greater than 1 ⁇ m, and this layer is subsequently silanized, if desired.
  • German patent document DE 10 2006 045 951 A1 relates to a method for the chemical modification and/or activation of the solid surfaces.
  • this method that employs at least one carrier medium, which is used to feed energy into the surface and to supply the surface with one or more halogen-containing compounds
  • the supply of the halogen containing compounds is carried out with a simultaneous addition of organosilicon compounds or silanes or organometallic compounds or silicon hydrides or metal hydrides to the carrier material.
  • An application which was filed by the same applicant and has the official application number 10 2010 054 473.6, relates to a method for promoting the adhesion of a surface of a titanium material.
  • the method generates an adhesion promoting layer, which is securely bonded to the surface of the titanium material and contains nanotubes, comprising titanium dioxide (TiO2), on the surface, and applies in an adherent manner an organic material to the adhesion promoting layer that comprises the nanotubes.
  • nanotubes comprising titanium dioxide (TiO2)
  • Exemplary embodiments of the present invention are directed to an alternative method that is designed to produce an adhesion promoting layer on a surface of a titanium material and for which the implementation requires only or at least predominantly environmentally compatible chemicals.
  • the method for producing an adhesion promoting layer on a surface of a titanium material comprises the introduction of the surface into an aqueous alkaline solution comprising sodium hydroxide at a concentration in a range from 100 to 300 g/l, sodium tartrate at a concentration in a range from 20 to 200 g/l, methyl glycine diacetic acid trisodium at a concentration in a range from 5 g/l to 60 g/l, and pentasodium triphosphate at a concentration in a range from 2 g/l to 20 g/l; and the application of a voltage between the solution and the titanium material for a predefined period of time, in order to produce the layer by means of anodic oxidation of the surface.
  • an aqueous alkaline solution comprising sodium hydroxide at a concentration in a range from 100 to 300 g/l, sodium tartrate at a concentration in a range from 20 to 200 g/l, methyl glycine diacetic acid triso
  • the sodium hydroxide is present preferably at a concentration in a range from 150 to 285 g/l, even more preferred 175 to 270 g/l, 195 to 250 g/l, 210 to 240 g/l, 238 to 242 g/l, and in particular 240 g/l.
  • the sodium tartrate is present preferably at a concentration in a range from 20 to 200 g/l, even more preferred 60 to 140 g/l, 75 to 125 g/l, 85 to 110 g/l, 90 to 105 g/l, and in particular 100 g/l.
  • the methyl glycine diacetic acid trisodium is present preferably at a concentration in a range from 10 to 50 g/l, even more preferred 15 to 40 g/l, 20 to 35 g/l, 25 to 33 g/l, 28 to 32 g/l, and in particular 30 g/l.
  • the pentasodium triphosphate is present preferably at a concentration of 3 to 17 g/l, even more preferred 4.5 to 13 g/l, or 6 to 10 g/l, or 7 to 8 g/l, or in particular 7.5 g/l.
  • any of the aforementioned concentration ranges or any concentration of one of the components of the solution can be combined with any concentration range or any other concentration of any other component.
  • an adhesion promoting layer formed as a layer of oxide can be created on the surface of the titanium material by means of anodic oxidation of the surface of the titanium material in the specified alkaline solution in such a way that the adhesion promoting layer exhibits adhesion promoting properties that are at least as good as those of the state of the art.
  • One advantageous feature is that exclusively or at least predominantly environmentally compatible active ingredients are necessary for this bonding purpose.
  • Sodium hydroxide contains Na+ ions that are known from conventional common salt.
  • Pentasodium triphosphate also known as triphosphate, is a component of biological compounds, such as adenosine triphosphate. In addition, pentasodium triphosphate is also approved as a food additive.
  • a particularly harmless substance i.e. methyl glycine diacetic acid trisodium, also known as the sodium salt of methyl glycine diacetic acid
  • a cleaning agent in particular, as a dishwashing detergent
  • Methyl glycine diacetic acid is also known by the name MGDA.
  • Sodium tartrate is a sodium salt of tartaric acid, also approved as a food additive and, therefore, also recognized as especially safe with respect to environmental considerations. The sodium tartrate acts in the alkaline solution as a titanium complexing agent and, as a result, can advantageously improve the redissolution properties.
  • the methyl glycine diacetic acid trisodium acts as an impurity ion complexing agent; and the pentasodium triphosphate acts as a skeleton former.
  • the alkaline solution is totally fluoride free and yet still allows an optimal pretreatment of the surface of the titanium material for a durable, high strength bonding between organic coatings.
  • the term titanium material may be understood to mean pure titanium or a titanium alloy, such as a titanium alloy, which is known as Ti6Al4V.
  • the anodic oxidation is carried out advantageously with a voltage in a range from 2 to 50 V, preferably 3 to 45 V, 5 to 35 V, 7 to 25 V, 9 to 20 V, 9 to 15 V, 10 to 12 V, and in particular 10 V.
  • the advantageous oxide layer can be generated at the specified voltage.
  • the anodic oxidation of the surface is carried out advantageously for a period of time, in which the advantageous adhesion promoting layer can be generated on the surface of the titanium material.
  • the duration of time is in a range from 5 to 60 min., preferably 8 to 50 min., 11 to 40 min., 15 to 30 min., 18 to 25 min., 19 to 22 min., and in particular 20 min.
  • Another embodiment of the method provides the anodic oxidation advantageously at a maximum current density, at which the advantageous adhesion promoting layer can be generated on the surface of the titanium material.
  • the maximum current density is in a range from 0.2 to 10 A/dm2, preferably 0.4 to 8 A/dm2, 0.6 to 4 A/dm2, 0.8 to 2 A/dm2, 1.0 to 1.5 A/dm2, 1.1 to 1.3 A/dm2, and in particular 1.2 A/dm2.
  • An additional embodiment of the method provides the anodic oxidation advantageously at a temperature, at which the advantageous adhesion promoting layer can be generated on the surface of the titanium material.
  • the temperature is in a range from 5 to 60° C., preferably 10 to 50° C., 15 to 40° C., 20 to 35° C., 25 to 33° C., 28 to 32° C., and in particular 30° C.
  • Another embodiment of the method provides an anodic oxidation of the surface in the alkaline solution and, as a result, the generation of an oxide layer having a layer thickness in a range from 50 to 600 nm, preferably 70 to 400 nm, 100 to 250 nm, and in particular 150 nm.
  • the advantage is that extremely good adhesion can be generated at the specified layer thickness.
  • Exemplary embodiments of the present invention are also directed to an adhesion promoting layer, which can be produced or is produced according to a method described above, on a surface of a titanium material as well as by means of a titanium material.
  • the surface of the titanium material has, in particular, a porous nanostructure with adjacent protrusions with undercuts, and, in particular, an interference color.
  • the individual structures are in the order of 50 to 300 nm.
  • the adhesion promoting layer on the surface of the titanium material can be coated and/or can be provided advantageously with an organic material for long term stability and with extremely good adherent properties.
  • it can also be detected by means of the interference color that the desired adhesion promoting layer is actually present on the surface of the titanium material or more specifically that the titanium material has the adhesion promoting layer on its surface.
  • the results are the advantages described above.
  • Exemplary embodiments of the present invention are also directed to the use of an aqueous alkaline solution with a method described above.
  • the results are the advantages described above.
  • FIG. 1 is a schematic view of a device for carrying out a method for anodic oxidization of a surface of a titanium material in an alkaline solution.
  • FIG. 2 is a plan view of an oxide layer, nano-structured by means of anodic oxidation, on the surface of a titanium material;
  • FIG. 3 shows a cryo-fracture of the surface, depicted in FIG. 2 , on the titanium material.
  • FIG. 1 shows a schematic view of a device 1 for producing an adhesion promoting layer on a surface 3 of a titanium material 5 .
  • the device 1 comprises a bath 7 with an electrolyte 9 .
  • the electrolyte 9 comprises sodium hydroxide, sodium tartrate, methyl glycine diacetic acid trisodium as well as pentasodium triphosphate in an aqueous solution.
  • the titanium material 5 and the bath 7 are connected to an electric energy source 11 . In so doing, an electric circuit is closed by way of the electrolyte 9 of the bath 7 .
  • the electric energy source 11 delivers a voltage 13 , which produces a current 15 in the electric circuit that is closed by way of the electrolyte 9 .
  • control and/or regulating devices (not shown in detail) for adjusting the voltage 13 and/or the current 15 may be provided.
  • the device 1 can be used to generate, by means of anodic oxidation, an oxide layer 17 (which is shown in FIGS. 2 and 3 ) on the surface 3 of the titanium material 5 .
  • the scales, shown in FIGS. 2 and 3 are drawn in each instance with a line that gives the length in nm.
  • the adhesion promoting layer is produced on the surface 3 of the titanium material 5 by means of anodic oxidization.
  • the surface 3 is introduced first into the bath 7 containing the alkaline solution or more specifically the electrolyte 9 , for example, by at least partially immersing the titanium material 5 in the electrolyte 9 .
  • the voltage 13 is produced between the electrolyte 9 and the titanium material 5 for a predefined period of time, in order to produce the layer by anodic oxidation of the surface 3 of the titanium material 5 .
  • FIG. 2 shows a plan view of the surface 3 of the titanium material 5 .
  • FIG. 3 shows a cryo-fracture of the titanium material 5 together with the surface 3 , and at the same time the oxide layer 17 can be seen.
  • a double arrow 19 in FIG. 3 symbolizes the thickness of the oxide layer 17 , where in this case the thickness is about 150 nm.
  • the oxide layer 17 has a distinct microporous nanostructure, which exhibits nodular growths that are arranged next to one another.
  • the nodular growths have a dimension of less than 300 nm, in particular less than 250 nm, in particular less than 200 nm, in particular less than 150 nm, preferably less than 50 nm to 100 nm and form an advantageous microporous surface.
  • the bath 7 is filled with the electrolyte 9 having a composition of 240 g/l of sodium hydroxide, 100 g/l of sodium tartrate, 30 g/l of methyl glycine diacetic acid trisodium, and 7.5 g/l of pentasodium triphosphate.
  • the surface 3 of the titanium material 5 is introduced, in particular immersed, at least partially in the bath 7 .
  • the voltage 13 of 10 V is applied to the at least partially immersed titanium material 5 and the bath 7 by means of the electric energy source 11 .
  • the current 15 is adjusted in such a way that the surface 3 of the titanium material 5 exhibits a current density of up to 1.2 A/dm2.
  • the voltage 13 and the current 15 and, thus, the current density of 1.2 A/dm2 are maintained for a duration of 20 minutes.
  • the bath 7 is kept at a specified temperature of 30° C.
  • devices for adjusting the temperature, for example, a heating unit and/or cooling system, may be provided in order to set the temperature to 30° C.
  • the desired nano structured surface 3 i.e. the oxide layer 17
  • the desired nano structured surface 3 can be obtained in a completely fluoride free process for the pretreatment of the titanium material 5 in order to achieve a durable, high strength bonding between the organic coatings.
  • Such a bonding can be achieved in an advantageous way by means of the micro-structured and/or nano-structured oxide layer 17 .
  • the described porous surface morphology can be generated advantageously on the titanium material 5 .
  • This titanium material can be coated in an adherent manner, for example, with organic materials, such as adhesives, paint, sealants and/or the like.
  • the electrolyte 9 is not only fluoride free, but also contains exclusively or at least predominantly environmentally compatible active ingredients that are particularly biodegradable.
  • the interference color can serve as proof that the treatment was carried out and/or can serve as an identifier for the respective treated components made of the titanium material 5 .
  • the oxide layer 17 on the surface 3 of the titanium material 5 can also be used for bonding biological material, for example, to implants.
  • the solution comprises ions of other components, in particular ions of the same period of a periodic table; and these ions are present at least in traces and/or as at least a partial substitution.
US14/130,817 2011-07-05 2012-07-13 Process for Producing an Adhesion-Promoting Layer on a Surface of a Titanium Material Abandoned US20140151235A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE201110106764 DE102011106764B4 (de) 2011-07-05 2011-07-05 Verfahren zur Herstellung einer haftvermittelnden Schicht auf einer Oberfläche eines Titanwerkstoffs durch anodische Oxidation , Verwendung einer Lösung für die anodische Oxidation und haftvermittelnde Schicht
DE102011106764.0 2011-07-05
PCT/IB2012/001944 WO2013005114A2 (de) 2011-07-05 2012-07-13 Verfahren zur herstellung einer haftvermittelnden schicht auf einer oberfläche eines titanwerkstoffs

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US (1) US20140151235A1 (de)
EP (1) EP2729604B1 (de)
DE (1) DE102011106764B4 (de)
WO (1) WO2013005114A2 (de)

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US20160312159A1 (en) * 2015-04-27 2016-10-27 Seacole-CRC, LLC Cleaning composition and method for processing equipment
US20210262097A1 (en) * 2018-06-29 2021-08-26 Airbus Operations Gmbh Preparation for pre-treating surfaces by chemically converting oxide layers of titanium or titanium alloys

Families Citing this family (2)

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DE102013017320A1 (de) * 2013-10-18 2015-04-23 Airbus Defence and Space GmbH Verfahren zum Trennen stoffschlüssig verbundener Materialien
RU2758704C1 (ru) * 2020-12-08 2021-11-01 Андрей Петрович Орлов Способ обработки тонких листов из титана

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Cited By (3)

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US20160312159A1 (en) * 2015-04-27 2016-10-27 Seacole-CRC, LLC Cleaning composition and method for processing equipment
US9963662B2 (en) * 2015-04-27 2018-05-08 Seacole-CRC, LLC Cleaning composition and method for processing equipment
US20210262097A1 (en) * 2018-06-29 2021-08-26 Airbus Operations Gmbh Preparation for pre-treating surfaces by chemically converting oxide layers of titanium or titanium alloys

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EP2729604A2 (de) 2014-05-14
DE102011106764B4 (de) 2013-03-14
WO2013005114A3 (de) 2013-04-04
WO2013005114A2 (de) 2013-01-10
DE102011106764A1 (de) 2013-01-10
EP2729604B1 (de) 2016-10-12

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