The purpose of this research was to study the synthesis of TiO2 

nanotubes on Ti-10Ta-10Nb thin film and the effect of applied potential 

on the tube size, length and morphology. The Ti-10Ta-10Nb thin film was 

deposited by dc magnetron sputtering on the CP Ti substrate. The 

anodization of this Ti-10Ta-10Nb thin film was performed in the solution

 containing 1M H3PO4 + 1.5wt.% HF at the potential readings of 4, 6, 8 

and 10 V for 10 minutes. The results showed that there was a slight 

increase in the tube diameter from approximately 25 nm at 4 V to 50 nm 

at 8 V. The length of nanotube varied from 700-900 nm. Interestingly, at

 the potential of 10 V, the nanotube diameters were damaged with slight 

decreases in nanotube lengths (500 nm)

Ahmad Ivan  Karayan

Deni  Ferdian

Yudha  Pratesa

International Journal of Technology

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International Journal of Technology (2012) 2: 181-185ISSN 2086-9614 © IJTech 2012SYNTHESIS OF TiO2 NANOTUBE ON TI-10Ta-10Nb THIN FILM BY ANODIZATIONAhmad Ivan Karayan, Deni Ferdian, Yudha PratesaCenter for Materials Processing and Failure Analysis (CMPFA), Department of Metallurgy andMaterials Engineering, Faculty of Engineering, Universitas Indonesia, Kampus Baru UI Depok 16424,Indonesia(Received: May 2011 / Revised: June 2011 / Accepted: July 2012)ABSTRACTThe purpose of this research was to study the synthesis of TiO2 nanotubes on Ti-10Ta-10Nbthin film and the effect of applied potential on the tube size, length and morphology. The Ti-10Ta-10Nb thin film was deposited by dc magnetron sputtering on the CP Ti substrate. Theanodization of this Ti-10Ta-10Nb thin film was performed in the solution containing 1MH3PO4 + 1.5wt.% HF at the potential readings of 4, 6, 8 and 10 V for 10 minutes. The resultsshowed that there was a slight increase in the tube diameter from approximately 25 nm at 4 V to50 nm at 8 V. The length of nanotube varied from 700-900 nm. Interestingly, at the potential of10 V, the nanotube diameters were damaged with slight decreases in nanotube lengths (500nm).Keywords: Anodization; Nanotube;  Synthesis; TiO21. INTRODUCTIONTi and Ti-based alloys have been widely used as implant materials due to their good mechanicalproperties and corrosion resistance. In the previous work, we studied the corrosion behaviour ofTi-8Ta-3Nb and Ti-10Ta-10Nb in comparison with CP Ti and Ti-6Al-4V (Karayan et al.,2008). The results showed that the corrosion resistance of Ti-10Ta-10Nb in simulatedphysiological media was superior to three other Ti based alloys, as characterized by Ti-10Ta-10Nb’s lowest passive current density.Kim et al., (2009) studied the cell adhesion of Ti-10Ta-10Nb and they reported that thesputtered nanoscale Ti-10Ta-10Nb coatings exhibited greater cell attachment compared to Ti-6Al-4V and Ti-10Ta-10Nb disks. A number of attempts have been extensively made tosynthesize TiO2 nanoporous on the titanium thin films (Mor et al., 2005; Xiaofeng et al., 2006)in order to increase the protein absorption in medical applications and light absorption in theenergy material applications. Unfortunately, no reports of nanoporous synthesis on Ti-Ta-Nbthin film could be found in the literature.The objective of this research was to study the synthesis of nanoporous formed on the Ti-10Ta-10Nb thin film and the effect of its potential on the pore size and morphology.2. METHODOLOGYThe Ti-10Ta-10Nb thin film was deposited on CP Ti substrate by using DC magnetronsputtering method within 4 hours at the bias voltage of – 300 V and power of 40 W. Thetemperature, gas pressure, and argon flow rate were set up at 300° C, 7.5 mTorr, and 30 sccm,respectively. Corresponding author’s email: deni@metal.ui.ac.id182 Synthesis of TiO2 Nanotube on Ti-10TA-10Nb Thin Film by AnodizationThe synthesis of nanotubes was performed by anodizing Ti-10Ta-10Nb – coated CP Ti in thesolution containing 1M H3PO4 + 1.5wt.% HF at the potentials of 4, 6, 8 and 10 V for 10minutes. The nanotubes formed on Ti-10Ta-10Nb thin film were characterized by scanningelectron microscope (SEM) and energy dispersive x-ray spectroscopy (EDS).3. RESULTS AND DISCUSSIONThe Ti-10Ta-10Nb thin film deposited by dc magnetron sputtering is shown in Figure 1.  Thisthin film with the thickness of approximately 964 nm was formed on the CP Ti substrate.Figure 1 Ti-10Ta-10Nb thin film with the thickness of 964 nm deposited on CP Tisubstrate by dc magnetron sputteringFigure 2 Size of nanotubes on Ti-z10Ta-10Nb thin film by anodization in the solutioncontaining 1M H3PO4 + 1.5wt.% HF at the applied potential of (a) 4 V, (b) 6 V, (c) 8 V and (d)10 Va bc dFerdian et al. 183The EDS spectrum of nanoporous , as shown in FigURE 3, showed the presence of Ti, Ta andNb, suggesting that the nanoporous was formed on the Ti-Ta-Nb thin films instead of CP Tisubstrate. A significant amount of titanium and oxide in the EDS spectrum might suggest thatthe nanoporous formed on Ti-10Ta-10Nb mainly composed of TiO2 along with a small amountof TaO and NbO. Further more detailed studies are needed to explore the type of metal oxidethat plays the most important role in nanoporous synthesis on Ti-10Ta-10Nb thin films.Informal transit services, which compete with regular buses was used as an alternative mode forcommuting. Even though informal transit services are illegal, they are necessary. Rather thanbanning informal transit services, transportation authorities could legalize and control theiroperations, providing a much needed additional (and more organized) commute mode.Figure 3 EDS spectrum of nanoporous formed on Ti-10Ta-10Nb thin film showing thepresence of Ti, Ta, Nb, O and F.The mechanism of metal nanotubes formation by anodization has been well documented (Sul etal., 2001; Chen et al, 2006; Grimes et al., 2009). With the onset of anodization a thin layer ofoxide forms on the titanium surface (Figure 4a). This oxide formation follows the reactionshown below Eequation 1) (Jaroenworaluck et al, 2007):Ti + 2H2O = TiO2 + 2H2 (1)The localized dissolution of TiO2 oxide leads to small pit formation, as represented by thereaction (3.2) (Lohrengel, 1993) and as shown in Figure 4b making the barrier layer at thebottom of the pits relatively thin which, in turn, increases the electric field intensity across theremaining barrier layer resulting in further pore growth, (Figure 4c).TiO2 + 6F- + 4H+ = TiF62- + 2H2O (2)The pore entrance is not affected by the electrical field assisted dissolution andhence remainsrelatively narrow, while the electrical field distribution in the curved bottom surface of the porecauses pore widening, as well as deepening of the pore [5]. The result is a pore with a scallopedshape (Sul et al., 2001; Chen et al., 2006; Grimes et al., 2009). As the Ti–O bond energy is high(323 kJ/mol), in the case of TiO2, it is reasonable to assume that only pores having thin wallscan be formed due to the relatively low ion mobility and relatively high chemical solubility ofthe oxide in the electrolyte, hence un-anodized metallic portions can initially exist between thepores. As the pores grow deeper the electrical field in these protruded metallic regionsincreases, enhancing field-assisted oxide growth and oxide dissolution, hence simultaneouslywith the well-defined pores, inter-pore voids start forming (Figure 4d). Thereafter, both voidsand tubes grow in equilibrium. The nanotube length increases until the electrochemical etchingrate equals the chemical dissolution rate of the nanotube top surface. After this point is reached,184 Synthesis of TiO2 Nanotube on Ti-10TA-10Nb Thin Film by Anodizationthe nanotube length will be independent of the anodization duration, as determined for a givenelectrolyte concentration and anodization potential (Grimes et al., 2009). Figure 4e shows thefully developed nanotubes with a corresponding top view.Figure 4 Schematic diagram of nanotube evolution at constant anodization voltage: (a)Oxide layer formation, (b) Pit formation on the oxide layer, (c) Growth of the pit intoscallop shaped pores, (d) The metallic region between the pores undergoes oxidation andfield assisted dissolution, (e) fully developed nanotubes with a corresponding top view(Mor et al., 2003).4. CONCLUSIONThe maximum potential for nanoporous synthesis of Ti-10Ta-10Nb by anodization in thesolution containing 1M H3PO4 + 1.5wt % HF was 8 V. We found that at this potential, thediameter of nanoporous was approximately 50 nm. The length of nanotubes varied from 700 –900 nm, with an exception at the potential of 10V where a slight decrease was noticed.5. REFERENCESChen, S.G., Paulose, M., Ruan, C., Mor, G.K., Varghese, O.K., Kouzoudis, D., Grimes, C.A.,2006. Electrochemically Synthesized CdS Nanoparticle-Modified TiO2 Nanotube-ArrayPhotoelectrodes: Preparation, Characterization, and Application to PhotoelectrochemicalCells, Journal of Photochemistry and Photobiology, Vol. 177, pp. 177–84Grimes, C.A. & Mor, G.K., 2009. TiO2 Nanotube Arrays: Synthesis, Properties, andApplications, Springer-Verlag Heidelberg, New York, USA.Jaroenworaluck, A., Regonini, D., Bowen, C.R., Stevens, R., Macro, D.A., 2007. Micro andNanostructure of TiO2 Anodised Flms Prepared in a Fuorine-Containing Electrolyte.Journal of Material Science, Vol. 42, pp. 6729–34.Ferdian et al. 185Karayan, A.I., Park, S.W., Lee, K.M., 2008. Corrosion Behavior of Titanium – Tantalum –Niobium Alloys in Simulated Physiological Media. Materials Letters, Elsevier, Vol. 62, pp.1843-5.Kim, Y.M., Vang, M.S., Yang, H.S., Park, S.W., Lim, H.P., 2009. Cell Response to a NewlyDeveloped Ti-10Ta-10Nb Alloy and Its Sputtered Nanoscale Coating. Journal of AdvancedProsthodontics, Vol. 1, No. 1, pp. 56-61.Lohrengel, M.M., 1993. Thin Anodic Oxide Layers on Aluminum and Other Valve MetalsHigh Feld Regime, Material Science and Engineering Report, Vol 11, pp. 243–94Sul, Y.T., Johansson, C.B., Jeong, Y., Albrektsson, T., 2001. The Electrochemical OxideGrowth Behaviour on Titanium in Acid and Alkaline Electrolytes. Medical Engineering andPhysics, Vol. 23, pp. 329–46.Mor, G.K., Varghese, O.K., Paulose, M., Mukherjee, N., Grimes, C.A., 2003. Fabrication ofTapered, Conical-Shaped Titania Nanotubes. Journal of Material Research, Vol.18, pp.2588–93.Mor, G.K, Varghese, O.K., Paulose, M., Grimes, C.A., 2005. Transparent Highly Ordered TiO2Nanotube Arrays via Anodization of Titanium Thin Films. Advanced Functional Materials,Vol. 15, No. 8, pp. 1291-6.Xiaofeng, Y., Yongxiang, L., Wanyin, G., Qunbao, Y., Nanfei, Z., Kourosh, K., 2006.Formation of Nanoporous Titanium Oxide Films on Silicon Substrates Using anAnodization Process. Nanotechnology, Vol. 17, No. 3.

Synthesis of TiO2 Nanotube in TI-10Ta-10Nb Thin Film by Anodization

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Synthesis of TiO2 Nanotube in TI-10Ta-10Nb Thin Film by Anodization

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