Precalcification Treatment of TiO2 Nanotube on Ti-6Al-4V Alloy

Si-Jung Kim; Ji-Man Park; Tae-Sung Bae; Eun-Jin Park

doi:10.4047/jkap.2009.47.1.39

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Kim, Park, Bae, and Park: Precalcification Treatment of TiO2 Nanotube on Ti-6Al-4V Alloy

ORIGINAL ARTICLE

J Korean Acad Prosthodont 2009;47(1):39-45.

Published online: 18 December 2009

DOI: https://doi.org/10.4047/jkap.2009.47.1.39

Precalcification Treatment of TiO2 Nanotube on Ti-6Al-4V Alloy

Si-Jung Kim, DDS¹, Ji-Man Park, DDS, MSD³, Tae-Sung Bae, PhD⁴, Eun-Jin Park, DDS, PhD, MSc^2,^∗

^¹Graduate Student, Department of Dental Prosthodontics, School of Medicine, Ewha Womans University

^²Assistant Professor, Department of Dental Prosthodontics, School of Medicine, Ewha Womans University

^³Graduate Student, Department of Prosthodontics, School of Dentistry, Seoul National University

^⁴Professor, Department of Dental Materials, School of Dentistry, Chonbuk National University

Corresponding Author: Eun-Jin Park Department of Dental Prosthodontics, School of Medicine, Ewha Womans University, 911-1 Mok-dong, Yangcheon-gu, Seoul, 158-710, Korea +82 2 2650 5042: e-mail, prosth@ewha.ac.kr

Received 29 November 200812 January 2009 Accepted 13 January 2009

This is an Open Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0/) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

Statement of problem

Recently precalcification treatment has been studied to shorten the period of the implant.

Purpose

This study was performed to evaluate the effect of precalcification treatment of TiO2 Nanotube formed on Ti-6Al-4V Alloy.

Material and methods

Specimens of 20 × 10 × 2 mm in dimensions were polished sequentially from #220 to #1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at 50℃ for 24 hours. The nanotubular layer was processed by electrochemical anodic oxidation in electrolytes containing 0.5 M Na2SO4 and 1.0 wt% NaF. Anodization was carried out using a regulated DC power supply (Kwangduck FA, Korea) at a potential of 20 V and current density of 30 ㎃/㎠ for 2 hours. Specimens were heat-treated at 600℃ for 2 hours to crystallize the amorphous TiO2 nanotubes, and precalcified by soaking in Na2HPO4 solution for 24 hours and then in saturated Ca(OH)2 solution for 5 hours. To evaluate the bioactivity of the precalcified TiO2 nanotube layer, hydroxyapatite formation was investigated in a Hanks’ balanced salts solution with pH 7.4 at 36.5℃ for 2 weeks.

Results

Vertically oriented amorphous TiO2 nanotubes of diameters 48.0 - 65.0 ㎚ were fabricated by anodizing treatment at 20 V for 2 hours in an 0.5 M Na2SO4 and 1.0 NaF solution. TiO2 nanotubes were composed with strong anatase peak with presence of rutile peak after heat treatment at 600℃. The surface reactivity of TiO2 nanotubes in SBF solution was enhanced by precalcification treatment in 0.5 M Na2HPO4 solution for 24 hours and then in saturated Ca(OH)2 solution for 5 hours. The immersion in Hank's solution for 2 weeks showed that the intensity of TiO2 rutile peak increased but the surface reactivity decreased by heat treatment at 600℃.

Conclusion

This study shows that the precalcified treatment of TiO2 Nanotube formed on Ti-6Al-4V Alloy enhances the surface reactivity. (J Korean Acad Prosthodont 2009;47:39-45)

Keywords: Implant surface, Anodization, Nanotube, Heat treatment, Precalcification, Surface activity

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Fig. 1.

FESEM images of TiO2 nanotubes anodized at 20 V for 2 hrs in 0.5 M Na2SO4 and 1 wt% NaF solution. (a) × 50 K; (b) × 100 K.

Fig. 2.

XRD patterns of TiO2 nanotubes. (a) anodized at 20 V; (b) heat-treated at 600℃.

Fig. 3.

XRD patterns of precalcified TiO2 nanotubes after immersed in SBF solution for 2 weeks. (a) Not heat - treated; (b) Heat-treated at 600℃.

Fig. 4.

SEM images of TiO2 nanotubes after immersed in Hanks’ solution for 2 weeks. (a) Not heat-treated; (b) Heat-treated at 600℃.

Fig. 5.

SEM images of precalcified TiO2 nanotubes after immersed in Hanks’ solution for 2 weeks. 3 K (a) and 10 K (b) of not heat-treated; 3 K (c) and 10 K (d) of heat-treated at 600℃.

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