# US 2014/0151235 A1 · Process for Producing an Adhesion-Promoting Layer on a Surface of a Titanium Material

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- Number: US 2014/0151235 A1
- Document ID: US20140151235A1
- Status: Published application
- Kind: A1
- Application number: 14/130,817
- Filed: 2012-07-13
- Published: 2014-06-05
- Earliest claimed: 2011-07-05
- Assignees: EADS Deutschland GmbH
- Inventors: Tobias Mertens; Franz Gammel
- Web page: https://patentgrep.com/patent/US20140151235A1

## CPC

- C25D 11/26: of refractory metals or alloys based thereon
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR

## Abstract

A method for producing an adhesion promoting layer on a surface of a titanium material involves introducing the surface into an aqueous alkaline solution of 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. A voltage is applied between the solution and the titanium material for a predefined period of time, in order to produce the layer by anodic oxidation of the surface.

## Claims

### Claim at position 1

1-13. (canceled)

### Claim 14

A method for producing an adhesion promoting layer on a surface of a titanium material, the method comprising:
introducing 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
applying a voltage between the solution and the titanium material for a predefined period of time, in order to produce the adhesion promoting layer by anodic oxidation of the surface.

### Claim 15 (depends on 14)

The method of claim 14, wherein the sodium hydroxide is present at a concentration in a range from 150 to 285 g/l.

### Claim 16 (depends on 15)

The method of claim 15, wherein the sodium hydroxide is present at a concentration in a range from 175 to 270 g/l, 195 to 250 g/l, 210 to 240 g/l, or 238 to 242 g/l.

### Claim 17 (depends on 16)

The method of claim 16, wherein the sodium hydroxide is present at a concentration of 240 g/l.

### Claim 18 (depends on 14)

The method of claim 14, wherein the sodium tartrate is present at a concentration in a range from 20 to 200 g/l.

### Claim 19 (depends on 18)

The method of claim 18, wherein the sodium tartrate is present at a concentration in a range from 60 to 140 g/l, 75 to 125 g/l, 85 to 110 g/l, or 90 to 105 g/l.

### Claim 20 (depends on 19)

The method of claim 19, wherein the sodium tartrate is present at a concentration of 100 g/l.

### Claim 21 (depends on 14)

The method of claim 14, wherein the methyl glycine diacetic acid trisodium is present at a concentration in a range from 10 to 50 g/l.

### Claim 22 (depends on 21)

The method of claim 21, wherein the methyl glycine diacetic acid trisodium is present at a concentration in a range from 15 to 40 g/l, 20 to 35 g/l, 25 to 33 g/l, or 28 to 32 g/l.

### Claim 23 (depends on 22)

The method of claim 22, wherein the methyl glycine diacetic acid trisodium is present at a concentration of 30 g/l.

### Claim 24 (depends on 14)

The method of claim 14, wherein the pentasodium triphosphate is present at a concentration of 3 to 17 g/l.

### Claim 25 (depends on 24)

The method of claim 24, wherein the pentasodium triphosphate is present at a concentration of 4.5 to 13 g/l, or 6 to 10 g/l, or 7 to 8 g/l.

### Claim 26 (depends on 25)

The method of claim 25, wherein the pentasodium triphosphate is present at a concentration of 7.5 g/l.

### Claim 27 (depends on 14)

The method of claim 14, wherein the anodic oxidation is carried out with a voltage in a range from 2 to 50 V.

### Claim 28 (depends on 27)

The method of claim 27, wherein the anodic oxidation is carried out with a voltage in a range from 3 to 45 V, 5 to 35 V, 7 to 25 V, 9 to 20 V, 9 to 15 V, or 10 to 12 V.

### Claim 29 (depends on 28)

The method of claim 28, wherein the anodic oxidation is carried out with a voltage of 10 V.

### Claim 30 (depends on 14)

The method of claim 14, wherein the anodic oxidation is carried out for a period of time in a range from 5 to 60 min.

### Claim 31 (depends on 30)

The method of claim 30, wherein the anodic oxidation is carried out for a period of time in a range from 8 to 50 min., 11 to 40 min., 15 to 30 min., 18 to 25 min., or 19 to 22 min.

### Claim 32 (depends on 31)

The method of claim 31, wherein the anodic oxidation is carried out for a period of time of 20 min.

### Claim 33 (depends on 14)

The method of claim 14, wherein the anodic oxidation is carried out at a maximum current density in a range from 0.2 to 10 A/dm2.

### Claim 34 (depends on 33)

The method of claim 33, wherein the anodic oxidation is carried out at a maximum current density in a range from 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, or 1.1 to 1.3 A/dm2.

### Claim 35 (depends on 34)

The method of claim 34, wherein the anodic oxidation is carried out at a maximum current density of 1.2 A/dm2.

### Claim 36 (depends on 14)

The method of claim 14, wherein the anodic oxidation is carried out at a temperature in a range from 5 to 60° C.

### Claim 37 (depends on 36)

The method of claim 36, wherein the anodic oxidation is carried out at a temperature in a range from 10 to 50° C., 15 to 40° C., 20 to 35° C., 25 to 33° C., or 28 to 32° C.

### Claim 38 (depends on 37)

The method of claim 37, wherein the anodic oxidation is carried out at a temperature of 30° C.

### Claim 39 (depends on 14)

The method of claim 14, wherein the anodic oxidation of the surface is carried out in the alkaline solution while generating an oxide layer having a layer thickness in a range from 50 to 600 nm.

### Claim 40 (depends on 39)

The method of claim 39, wherein the anodic oxidation of the surface is carried out in the alkaline solution while generating an oxide layer having a layer thickness in a range from 70 to 400 nm or 100 to 250 nm.

### Claim 41 (depends on 40)

The method of claim 40, wherein the anodic oxidation of the surface is carried out in the alkaline solution while generating an oxide layer having a layer thickness of 150 nm.

### Claim 42

An adhesion promoting layer on a surface of a titanium material, the adhesion promoting layer being producible or produced by introducing 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 applying a voltage between the solution and the titanium material for a predefined period of time, in order to produce the adhesion promoting layer by anodic oxidation of the surface, wherein the adhesion promoting layer has a porous nanostructure with adjacent protrusions with undercuts as well as an interference color.