effect of storage temperature on ti-6al-4v surface wettability
DESCRIPTION
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 - PowerPoint PPT PresentationTRANSCRIPT
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
22
Motivation and Background
Titanium and Alloys
• Corrosion resistance, mechanical properties and biocompatibility
• Numerous biomedical applications– Dentistry– Orthopaedics– Cardiovascular– Ophthalmology
2Figure from Geetha Manivasagam et al. Biomedical Implants: Corrosion and its Prevention - A Review. Recent Patents on Corrosion Science. 2010, pp. 40-54. 3
Osseointegration
• Connection between the implant and the living bone• Prevention of implant loosening
3Figure 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
Water adsorption Proteins adsorption Cells adsorption
Water Dissociation on TiO2 Surface
3Figure adapted from Z. Zhang et al. Imaging Water Dissociation on TiO2(110): Evidence for Inequivalent Geminate OH Groups J. Phys. Chem. B 2006, 110, 21840-21845 5
(a) TiO2 surface with oxygen vacancy(b) Two hydroxyl groups HV (at a vacancy) and HB (protonation of
neighbor oxygen atom) formed by water adsorption and dissociation (c) HB diffusion
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
6
200 °C 400 °C 600 °C0
1020304050607080
Samples stored in glass Petri-dish in air
Day 0Day 1Day 2Day 3Day 4Day 5Day 8Day 9
Thermally oxidized samples
Ave
rage
Wat
er C
onta
ct A
ngle
(°)
Evolution of water contact angle – Samples stored in glass petri –dish in air (Data acquisition and graph preparation by
Sweetu Patel)
6
Samples in current storage conditions
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
7
[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. Photocatalysis on TiOn Surfaces: Principles, Mechanisms, and Selected Results . Chem. Rev. 1995, 95, 735-758. 7
Sample Preparation
Sample Preparation
• Sandblasting – 50 µm alumina grit particles– 517 kPa
28
• Acid Etching
Figure from L.G. Harris, et al.Staphylococcus aureus adhesion to titanium oxide surfaces coated with non-functionalized and peptide-functionalized poly(l-lysine)-grafted-poly(ethylene glycol) copolymers , Biomaterials, Volume 25, Issue 18, August 2004
H2SO4 + H2O2 → H2SO5 + H2O
Sample Preparation
• Sonication – 1 hour methanol (99.8%)
• Wash – 30 seconds deionized water (DI-water)
• Annealing – 3h in air
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AnnealingScheme (adapted from http://www.memsnet.org/mems/processes/deposition.html)
Not Annealed
400 ºC
600 ºC
Annealing Storage Condition
Group 1
Not Annealed
Kimwipe
Group 2 Room Temp. DI-Water
Group 3 Cold DI-Water*
Group 4
400 ºC
Kimwipe
Group 5 Room Temp. DI-Water
Group 6 Cold DI-Water*
Group 7
600 ºC
Kimwipe
Group 8 Room Temp. DI-Water
Group 9 Cold DI-Water*
10*Refrigerator temperature: 8 ± 2 ºC
Surface Characterization
Zygo
411
Roughness (µm)Not Annealed 400 ºC 600 ºC
RMS 2.27 ± 0.27 2.57 ± 0.47 2.51 ± 0.56
Sample 45 surface
FTIR
412
• Infrared Spectrum (absorbance)
• Deconvolution using XPSpeak
Figure from http://www.bgtu.net/image/ik.jpg
13
14
15
Anatase
Ti-O bond
16
17
RutileV-O
Al2O3
18
Al2O3
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
419
20
0 5 10 15 20 25 30 350
20
40
60
80
100
120
140
160
Samples Not AnnealedGroups 1, 2 and 3
Kimwipe Room Temperature Water Cold Water
Time (days)
Wat
er C
onta
ct A
ngle
(º)
Cold water samples warmed up to room temperature
Samples immersed in water and warmed up to 37 ºC
21
0 5 10 15 20 25 30 350
20
40
60
80
100
120
140
160
Samples Annealed at 400 ºCGroups 4, 5 and 6
Kimwipe Room Temperature Water Cold Water
Time (Days)
Wat
er C
onta
ct A
ngle
(º)
Cold water samples warmed up to room temperature
Samples immersed in water and warmed up to 37 ºC
22
0 5 10 15 20 25 30 350
20
40
60
80
100
120
140
160
Samples Annealed at 600 ºCGroups 7, 8 and 9
Kimwipe Room Temperature Water Cold Water
Time (Days)
Wat
er C
onta
ct A
ngle
(º)
Cold water samples warmed up to room temperature
Samples immersed in water and warmed up to 37 ºC
23
Conclusions
• Best annealing temperature: 600 ºC– Rutile formation– Signatures related to vanadium and aluminum oxides from FTIR
spectrum
Water Contact Angle After 34 Days (º) Not Annealed 400 ºC 600 ºC
Kimwipe 61 ± 10 54 ± 10 31 ± 13
Room Temperature Water 12 ± 4 12 ± 4 7 ± 2
Cold Water 9 ± 3 12 ± 4 4 ± 2
24
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. Zhang et al. Imaging Water Dissociation on TiO2(110): Evidence for Inequivalent Geminate OH Groups J. Phys. Chem. B 2006, 110, 21840-21845
Acknowledgments
AMReLAdvanced Materials Research Laboratory
ORTHOPAEDIC AND DENTAL RESEARCH GROUP
RUSH, Michigan Tech and UIC
Dr. Gregory Jursich, Sweetu Patel, Azhang Hamlekhan and Dmitry Royhman
Questions? Comments?