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Received January 27, 2006
Accepted July 4, 2006
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Hydrothermal synthesis of titanate nanotubes followed by electrodeposition process
Thin Film Technology Laboratory, School of Chemical Engineering, Chonbuk National University, Jeonju 561-756, Korea
hsshin@chonbuk.ac.kr
Korean Journal of Chemical Engineering, November 2006, 23(6), 1037-1045(9), 10.1007/s11814-006-0027-x
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Abstract
Titanate nanotubes were synthesized by hydrothermal process using commercial titania nanoparticles. The experiments were carried out as a function of reaction time, temperature, and NaOH concentration. Furthermore, the titanate nanotube film was fabricated on the Si substrate using electrodeposition method with 60 V and at room temperature. The specimens were investigated by using various techniques such as field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman Spectroscopy, and Xray photoelectron spectroscopy (XPS). The formation of sodium titanate nanotubes was affected strongly by the variation in all parameters. The best conditions for the titanate nanotubes were found to be a reaction temperature of 150 ℃, 10 M NaOH concentration, and reaction time of 48 hr. Under the best conditions, the resulting titanate nanotubes did not contain any remains of starting material, namely P25 nanoparticles, and also the resulting nanotubes had very smooth morphology with a diameter of ~10 nm and length extending up to several micrometers without presence of any bundlelike structures. The washing of sodium titanate nanotubes with HCl solution leads to conversion into protonic titanate nanotubes via ion exchange reaction. The subsequent sintering of the titanate nanotubes renders dehydration of interlayered OH groups, thereby leading to precipitation of anatase phase. The tubular structure also gets destroyed during phase change, beyond 375 ℃. The electrodeposited titanate film with 60 V for 10 min at room temperature was dense and uniform. In this work, we suggest that electrochemical deposition method of titanate nanotubes film can be used for its applications.
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