Titanium dioxide (TiO2) nanotube photocatalyst is highly desired for the photodegradation of dye in wastewater treatment. A series of titanium dioxide nanotube photocatalysts were successfully synthesized using methylamine as N-ligand via hydrothermal treatment at different hydrothermal temperatures and durations. The effect of these two parameters on the photocatalytic activity of synthesized materials were investigated. TEM micrographs and XRD analysis depicted methylamine assisted the transformation of anatase TiO2 nanoparticles to nanotube via the exfoliation of TiO2 crystallite into layered sheet and promoted the curling of layered sheet. Hydrothermal temperature up to 180°C was able to fully transform the morphology of anatase TiO2 nanoparticles into nanotube. The reaction duration was further modified. Fluorescence analysis showed that 24 h hydrothermal duration gave the slowest electron-hole recombination rate. DR-UV-Vis analysis indicated that the synthesized samples were active under UV region. The photocatalytic performance of the synthesized materials was tested in the photodegradation of Congo red under UV irradiation. The results suggested that among the materials synthesized, TiO2 nanotube synthesized at 180°C, under 24 h hydrothermal duration appeared to be the most superior photocatalyst which gave the highest photocatalytic activity of 77%. Possible mechanism of the TiO2 nanotube formation with methylamine as N-ligand is presented.
Titanium dioxide (TiO2) nanotubes (TNT) were successfully synthesized using different N-containing ligands via hydrothermal method. Methylamine, ethylenediamine and diethylenetriamine with different Ti/ligand molar ratios (1:1, 1:3, 1:5 and 1:8) were prepared. As-synthesized TiO2 without N-containing ligands were also prepared for comparison purpose. The X-Ray Diffraction patterns confirmed the presence of anatase phase of TiO2 in all the synthesized samples whereas the presence of sodium titanate was only detected in the samples containing N-containing ligands. The Transmission Electron Microscopy images also showed that the N-containing ligands promoted the formation of nanotubes in the anatase TiO2. Based on the Tauc Plot, the band gap energy of anatase TiO2 was shifted with the addition of methylamine, ethylenediamine and diethylenetriamine. The photoluminescence spectra also showed that with the addition of sufficient amount of N-containing ligands, the intensity of photoluminescence spectrum decreased, suggesting formation of more nanotube and reduction of electron hole recombination rate. The photocatalytic performance of all synthesized samples was determined through photodegradation of Congo red under UV light for 6 hours. The results suggested that among the synthesized materials, the sample which contained diethylenetriamine with molar ratio of 5 gave the highest photocatalytic activity of 76.71% which could be attributed to successful formation of nanotube, its higher surface rate reaction and low electron hole recombination. Diethylenetriamine showed higher efficiency in assisting the formation of TiO2 nanotubes compared to methylamine and ethylenediamine.
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