npsm 새물리 New Physics : Sae Mulli

pISSN 0374-4914 eISSN 2289-0041


Research Paper

New Physics: Sae Mulli 2014; 64: 723-730

Published online July 31, 2014

Copyright © New Physics: Sae Mulli.

Fabrication of P- and Ca-doped Ti Nanotube Arrays by Using Anodization

양극산화 방법으로 제조한 P와 Ca가 도핑된 TiO$_{2}$ 나노튜브 박막

Kun Ho KIM*1, Jeoung Ju LEE1, Sung Am CHO2

1 Department of Physics and RINS, Gyeongsang National University, Jinju 660-701, Korea
2 Department of Prosthodontics, College of Dentistry, Kyungpook National University, Daegu 700-412, Korea


Received: April 30, 2014; Revised: June 25, 2014; Accepted: June 26, 2014

This is an open-access article distributed under the terms of the Creative Commons Attribution Non-Commercial License ( which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.


In this study, highly-ordered TiO$_{2}$ nanotube (TNT) arrays were fabricated by using electrochemical anodization of Ti-foil in ethylene glycol electrolytes containing 0.4 wt% $\sim$ 1 wt% NH$_{4}$F and about 2 vol% H$_{2}$O. Sodium glycerophosphate (0.3 mol%) and calcium acetate (0.02 mol%) were added in the electrolyte as Ca- and P- doping sources. Anodization was carried out at current density of about 20 to 150 mA/cm$^{2}$ for about 30 to 120 min. Well-ordered TNT arrays with average diameters from 50 to 120 nm and lengths from about 0.3 to about 1.5 $\mu$m were fabricated. The anatase TiO$_{2}$ phase was formed by annealing at 400 $^\circ$C, it was changed to the rutile TiO$_{2}$ phase by annealing at 600 $^\circ$C and it was transformed to the rutile phase completely by annealing at 800 $^\circ$C. Energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analyses showed that the overall doping level of P was 2.2 $\sim$ 4.6 at% and that of Ca was 5.8 $\sim$ 6.8 at%. We believe that our method for fabricating Ca- and P- doped TNT arrays on Ti plates is an effective method and is applicable to the development of TNT-based dental implants.

Keywords: TiO$_{2}$ nanotube, Anodization, P doping, Ca doping, Honeycomb structure

약 2 vol%의 물을 포함한 ethylene glycol에 약 0.4 wt% $\sim$ 1 wt%의 NH$_{4}$F를 용해시킨 다음 0.3 mol%의 sodium glyeorophosphate 및 0.02 mol% calcium acetate를 첨가한 용액을 사용하여 양극산화 방법으로 P와 Ca가 도핑된 TiO$_{2}$ 나노튜브 박막을 제조하였다. 전류밀도 20 mA/cm$^{2}$ $\sim$ 150 mA/cm$^{2}$에서 30분에서 120분간 성장시켜 직경 50 nm$\sim$150 nm 범위, 길이 약 0.3 $\mu$m $\sim$ 1.5 $\mu$m에 이르는 나노튜브 array를 형성하였다. 형성된 나노튜브 array는 비정질이었으나 400 $^\circ$C에서 열처리함에 따라 anatase 상, 그리고 600 $^\circ$C 이상의 온도에서 rutile 상으로 상전이하였으며, 800 $^\circ$C 이상에서는 완전히 rutile 상으로 전이되었다. 에너지 분산 X-선 분광법 (EDS)과 광전자 분광법 (XPS)을 통해 나노튜브 내에 약 2.2 at% 에서 4.6 at%의 P와 5.8 at%에서 6.8 at%의 Ca이 도핑되어 있음을 확인하였다. 제작된 TiO$_{2}$ 나노튜브 어레이는 직경, 길이, 치밀도 그리고 상 (phase) 등 치과용 Ti 임플란트에 적용할 수 있을 것으로 기대되는 구조적 특성을 지니고 있었다.

Keywords: TiO$_{2}$ 나노튜브, 양극산화, P, Ca 도핑, 벌집 구조

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