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Effect of Storage Temperature on Ti-6Al-4V Surface Wettability. Caio Peixoto*, Arman Butt** and Christos Takoudis** *Federal University of Rio Grande do Norte **University of Illinois at Chicago. Outline. Motivation and Background Sample Preparation Surface Characterization
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Effect of Storage Temperature on Ti-6Al-4V Surface Wettability Caio Peixoto*, Arman Butt** and Christos Takoudis** *Federal University of Rio Grande do Norte **University of Illinois at Chicago
Outline • Motivation and Background • Sample Preparation • Surface Characterization • Roughness (Zygo) • Chemistry (Fourier Transform Infrared Spectroscopy – FTIR) • Wettability (Water Contact Angle) • Conclusions 2 2
Titanium and Alloys • Corrosion resistance, mechanical properties and biocompatibility • Numerous biomedical applications • Dentistry • Orthopaedics • Cardiovascular • Ophthalmology Figure from GeethaManivasagam et al. Biomedical Implants: Corrosion and its Prevention - A Review. Recent Patents on Corrosion Science. 2010, pp. 40-54. 3 2
Osseointegration • Connection between the implant and the living bone • Prevention of implant loosening Cells adsorption Water adsorption Proteins adsorption Figure adapted from M. Geetha et al.Ti based biomaterials, the ultimate choice for orthopaedic implants - A review. Pregress in Materials Science. 2009, pp. 397-425. 4 3
Water Dissociation on TiO2 Surface • TiO2 surface with oxygen vacancy • Two hydroxyl groups HV (at a vacancy) and HB (protonation of neighbor oxygen atom) formed by water adsorption and dissociation • HB diffusion Figure adapted from Z. Zhanget al.Imaging Water Dissociation on TiO2(110): Evidence for Inequivalent Geminate OH Groups J. Phys. Chem. B 2006, 110, 21840-21845 5 3
Motivation • Current storage method: samples in air (Petri-dish or Kimwipe • Decrease in wettability over time • Materials can be mistakenly classified as bad by further tests Evolution of water contact angle – Samples stored in glass petri –dish in air (Data acquisition and graph preparation by Sweetu Patel) Samples in current storage conditions 6 6
Background • Surface wettability decreases over time due to poor storage methods1 • At 2x10-10 Torr, increase in temperature results in water desorption and hydroxyl group loss2 [1] Jung Hwa Park et al. Effect of cleaning and sterilization on titanium implant surface properties and cellular response. Acta Biomaterialia, 2011 [2] Amy L. Linsebigler, et al. PhotocatalysisonTiOnSurfaces: Principles, Mechanisms, andSelectedResults. Chem. Rev. 1995, 95, 735-758. 7 7
Sample Preparation • Acid Etching • Sandblasting • 50 µm alumina gritparticles • 517 kPa • H2SO4 + H2O2 → H2SO5 + H2O Figure from L.G. Harris, etal.Staphylococcusaureusadhesion to titanium oxide surfacescoatedwithnon-functionalizedandpeptide-functionalizedpoly(l-lysine)-grafted-poly(ethyleneglycol) copolymers, Biomaterials, Volume 25, Issue 18, August 2004 8 2
Sample Preparation • Sonication – 1 hour methanol (99.8%) • Wash – 30 seconds deionized water (DI-water) • Annealing – 3h in air Not Annealed 400 ºC 600 ºC AnnealingScheme(adapted from http://www.memsnet.org/mems/processes/deposition.html) 9 2
Zygo Sample 45 surface 11 4
FTIR • Infrared Spectrum (absorbance) • Deconvolution using XPSpeak 12 Figure from http://www.bgtu.net/image/ik.jpg 4
Anatase Ti-Obond 15
V-O Rutile Al2O3 17
Al2O3 18
Water Contact Angle • Water contact angle measurements • After 0h, 3h, 6h,12h, 1d, 2d, 6d, 9d,13d, 16d and 20d • Cold water groups let to warm up to room temperature • Measurements after 20d3h, 20d6h, 20d12h, 21d, 23d and 27d • Warm up all the samples to 37 °C • Measurements after 27d3h, 27d6h, 27d12h, 28d, 30d, 34d 19 4
Samples immersed in water and warmed up to 37 ºC Cold water samples warmed up to room temperature 20
Samples immersed in water and warmed up to 37 ºC Cold water samples warmed up to room temperature 21
Samples immersed in water and warmed up to 37 ºC Cold water samples warmed up to room temperature 22
Conclusions • Best annealing temperature: 600 ºC • Rutile formation • Signatures related to vanadium and aluminum oxides from FTIR spectrum 23
Conclusions • Best storage condition: immersed in DI-water • Storage temperature showed no major effect • Samples wrapped in Kimwipe decreased drastically when immersed in DI-water • Water dissociation reaches equilibrium Figure adapted from Z. Zhanget al.Imaging Water Dissociation on TiO2(110): Evidence for Inequivalent Geminate OH Groups J. Phys. Chem. B 2006, 110, 21840-21845 24
Acknowledgments AMReLAdvanced Materials Research Laboratory Orthopaedic and Dental Research Group RUSH, Michigan Tech and UIC Dr. Gregory Jursich, Sweetu Patel, AzhangHamlekhanandDmitryRoyhman