Surface Treatment of Titanium

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1 Surface Treatment of Titanium Christiane Jung KKS Ultraschall AG, Steinen SZ The Tribology of Precision Swiss Tribology Meeting SBB Centre Löwenberg in Murten, Switzerland 16. November

2 Outline: 1. KKS Ultraschall AG 2. Surface Treatment of Titanium 2

3 3

4 KKS-Ultraschall AG Ultrasonic & Surface Technologies Profile - Development and Production of Cleaning Units based on Ultrasonic Technology. - Surface Finish and Cleaning of Metal Parts, in particular of Implants made from Titanium and Stainless Steel. History 1982: Foundation of the Company KKS Keller H.P. 1999: Change to an Aktiengesellschaft KKS Ultraschall AG Ultraschall & Oberflächentechnik 2006: New Building Medical Surface Center 2007: 25 Anniversary Coworkers: ~ 55 (2007) 4

5 2005 Medical Surface Center

6 Products Units for Surface Treatment and Cleaning Small Ultrasonic Bath, Liter Dry-Blasting Units Unit for Electropolishing Ultrasonic Vibrators Ultrasonic Generators One-Chamber Ultrasonic Unit (Cleaning, Rinsing, Drying) Automated Cleaning Unit (Cleaning, Rinsing, Passivation, Drying) 6

7 Services Titanium Stainless steel Metals 7

8 Medical Surface Center Surface Treatment of Implants and Instruments made from Titanium and Titanium Alloys 8

9 Titanium Surface properties are important! 9

10 The PDF-Effect of the Surface Surface Treatment 1. Protective effect (P) - chemical resistance; friction; wear; hardness;. 2. Decorative effect (D) - color; brightness; haptic. 3. Functional effect (F) - improvement of the interaction with other materials (i.e. metals, polymers, biological tissues, bone ) 10

11 Outline: 2. Surface Treatment of Titanium 2.1. Passive Layer 2.2. Color-Anodizing (KKS01, TioCol) 2.3. Importance of Mechanical Pretreatment (KKS00) for the Quality of Color-Anodized Surfaces 2.4. Dark-Anodizing (KKS02, TioDark) 11

12 The natural passive layer Titanium + Oxygen Titanium dioxide (natural oxidation) [ Ti ] + [ O 2 ] [ TiO 2 ] Titanium dioxide passive layer (TiO 2 ) (~ 5 nm thickness) titanium substrate 12

13 The artificial passive layer natural passive layer artificial passive layer titanium substrate titanium substrate Chemical Oxidation Oxidizing agents such as: Nitric acid (HNO 3 ) Hydrogen peroxide (H 2 O 2 ) Thickness < 40 nm Thermal Oxidation Electrochemical Oxidation ( Anodizing ) 13

14 Electrochemical Oxidation ( Anodizing ) Protective Effect Thicker passive layer (up to ~ 300 nm) Protection against further corrosion. Decorative Effect Functional Effect Color-Anodizing TioCol 14

15 2.2. Color-Anodizing (KKS01, TioCol) start Electrochemical cell 15

16 2.2. Color-Anodizing (KKS01, TioCol) step 1 Electrochemical cell 16

17 2.2. Color-Anodizing (KKS01, TioCol) step 2 Electrochemical cell 17

18 Increase of layer thickness changes the color due to light ray interference. Gasoline on water 18

19 Colors are used as codes for implants and tools. 19

20 Electrochemical Cells Medical Surface Center 20

21 2.4. Importance of mechanical pretreatment ( KKS00 ) for the quality of color-anodized surfaces grinding media High brightness of the surfaces Surface roughness R a ~ µm Side-view topography 21

22 Microcrystals acting as grinding and polishing particles? microscopic images; magnification

23 Pretreatment with small-sized granulate combines mechanical with chemical treatment? Magnification 63 ph ~ 5 Granulate impregnated with wax, plant and mineral oils, fatty acids, emulsifier, and oxides as grinding particles 23

24 Surface Roughness of Titanium Discs (polished with granulate) before anodizing sr a = µm Ti 6Al 7Nb color-anodized at 62 V sr a = µm 24

25 2.4. Dark-Anodizing (KKS02, TioDark) Electrochemical cell 25

26 Main steps for Dark-Anodizing (KKS02, TioDark) Start Color formation Oxygen evolution Sparking Increasing voltage Porous outermost layer Conversion layer Titanium substrate 26

27 Raster Electron Microscopic Picture (cpti, grade 2) Porous outermost layer Conversion layer Titanium substrate before anodizing 27

28 Examples for dark-anodized titanium surfaces ( TioDark ) (Ti 6Al 4V, porous layer removed) before after before after before before after after 28

29 Surface Topography of untreated and dark-anodized Ti 6 Al 4 V - samples before after sr a = µm sr a = µm Surface roughness for different samples of cpti (grade 2 & 4), Ti6Al4V, Ti6Al7Nb) before after sr a ~ µm 29

30 Surface characterization by Raman spectroscopy Suggested assignment: Contributions of: Rutile TiO 2 Anatase TiO 2 30

31 31

32 Scratch test dark-anodized sample scratches color-anodized sample (Ti 6Al 4V / Ti 6Al 4V - pair) Surface of dark-anodized sample Magnification 63 Ti 6Al 4V Scratch spots: Magnification: 63 expected color in scratch spot 32

33 Scratch test (diamond / cpti grade 4 - pair) Diamond cone 90 ; velocity: 0.1 mm/s; distance: 5 mm; zero load: 1.0 mn; load: 20 mn; load cycles: 10 33

34 Friction: Steel/Titanium Pair Dependence of the friction coefficient on the sliding distance CSM: standard tribometer, ball on disc method ball: steel 100Cr6 34

35 Initial friction coefficient sliding distance = 6.7 mm, scaled to untreated surfaces CSM standard tribometer ball: steel 100Cr6, 6mm, dry; linear mode, ½ amplitude: 2mm, max linear speed: 2 cm/s, normal load: 250 mn, cycles: 470, acquisition rate: 10 Hz, temperature: 25 C, atmosphere: air, huminity: 35% CSM: standard tribometer, ball on disc method 35

36 Initial friction coefficient scaled to untreated surfaces Steel/Titanium Pair Comparison: CSM nano tribometer (20 mn load) and standard tribometer (250 mn load) CSM nano tribometer 36

37 Nano- and micro-hardness of dark-anodized surfaces. Indentation profil 37

38 Summary TioDark Lower initial friction coefficient. Increased micro- and nano-hardness. Increased layer thickness. Very good haptic. Dense, dark and low-reflective Biocompatible compared to untreated surfaces 38

39 Surface Treatment A great challenge 39

40 Acknowledgement CSM (Micro- and nano-hardness; tribology studies) INNOWEP (Nano-scratch test, wear rate) CSEM (Thickness measurements) SGS Institute Fresenius (XPS depth profile analysis) Fachhochschule der Nordwestschweiz (REM/EDX) Technical University Berlin, Institute for Chemistry (Raman spectroscopy) FRT Suisse AG (Surface topography analysis) 40

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