Electrochemical synthesis and characterization of titania nanotube thin film
Titania nanotubes (TNT) have gained increasing interest due to their high surface area, fewer interfacial grain boundaries and excellent charge transfer between interfaces; all are critical properties in photoelectrochemical and photocatalysis application. In this study, TNT thin film electrodes wer...
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| Format: | Thesis |
| Language: | English |
| Published: |
2013
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| Online Access: | http://psasir.upm.edu.my/id/eprint/67431/1/FS%202013%2062%20IR.pdf http://psasir.upm.edu.my/id/eprint/67431/ |
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| Summary: | Titania nanotubes (TNT) have gained increasing interest due to their high surface area, fewer interfacial grain boundaries and excellent charge transfer between interfaces; all are critical properties in photoelectrochemical and photocatalysis application. In this study, TNT thin film electrodes were synthesized by electrochemical anodisation of pure Ti in a standard two-electrode cell containing NH4F solution. Parameters affecting the morphological, structural and geometry of TNT were investigated in three different electrolytic medium namely the acidic aqueous solution (NH4F/H2O), mixture of aqueous-organic solution (NH4F/H2O/EG) and an organic neutral solution (NH4F/EG).
The characteristic of TNT were analyzed using Field Emission Scanning Electron Microscopy (FESEM), X-ray Diffractometry (XRD), Transmission Electron Microscopy (TEM), Energy Dispersive X-ray Analysis (EDX) and UV Visible Diffuse Reflectance Spectroscopy (UV-DRS). Meanwhile, the photoelectrochemical responses of TNT were investigated using Liner Sweep Photovoltammetry (LSPV) and their photoefficiency was evaluated in 0.1 M KOH under UV illumination. The thermal stability of short TNT (400 nm in length) and its morphological, structural,
optical and photoelectrochemical changes as a result of heat treatment at 200-800 oC
were also studied.
In NH4F/H2O electrolyte, sample morphology was affected by electrolyte pH and
fluoride concentration whereby nanotubes dimensions and their growth rate can be
manipulated via anodisation voltage, bath temperature, anodisation duration and the
addition of EDTA. Voltage range and NH4F concentration used for TNT formation
varied depending on the electrolytic medium used during anodisation. Higher voltage
range could be used in NH4F/EG to obtain larger diameter and longer length tube. An
optimum fluoride concentration is required to achieve well-defined and long tube as
higher amount of F- leads to faster chemical dissolution.
Choice of electrolytic medium also has an influence on the crystalline structure,
regularity, morphology, elemental composition and band gap of TNT. XRD results
showed that pure anatase phase was obtained in NH4F/EG/H2O and NH4F/EG
solution while mixture of anatase and rutile co-existed for TNT prepared in
NH4F/H2O solution. As opposed to irregular nanotubes with ripples formed in
NH4F/H2O, regular and smooth TNT with variation in length were obtained in
NH4F/EG.
The as-anodised TNT is amorphous and transformed to anatase phase at 300 oC.
Crystallization of anatase phase increases on elevating calcination temperature and
rutile phase co-existed at 500 oC. TNT is thermally stable up to temperature < 600 oC,
above which changes in morphology and dimensions of TNT occurred. Calcination of TNT at 500 oC appeared to be the most favorable condition to retain the nanotubular
structure with desired crystal phase and photoelectrochemical properties.
The morphology and geometry of the TNT are important factors influencing the
photoelectrochemical response, with higher photocurrent response are generally
associated with thicker layer of TNT. Photoefficiency for TNT synthesized in
different electrolytes medium was tested under halogen and UV light illumination.
Highest photoefficiency was obtained for TNT prepared in NH4/EG compared to
those prepared in other electrolytes due to formation of longer length tube. |
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