Rapid breakdown anodization technique for the synthesis of high aspect ratio and high surface area anatase TiO2 nanotube powders

Clusters of high aspect ratio, high surface area anatase-TiO2 nanotubes with a typical nanotube outer diameter of about 18 nm, wall thickness of approximately 5 nm and length of 5–10 μm were synthesized, in powder form, by breakdown anodization of Ti foils in 0.1 M perchloric acid, at 10 V (299 K) and 20 V (∼275 and 299 K). The surface area, morphology, structure and band gap were determined from Brunauer Emmet Teller method, field emmission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman, photoluminescence and diffuse reflectance spectroscopic studies. The tubular morphology and anatase phase were found to be stable up to 773 K and above 773 K anatase phase gradually transformed to rutile phase with disintegration of tubular morphology. At 973 K, complete transformation to rutile phase and disintegration of tubular morphology were observed. The band gap of the as prepared and the annealed samples varied from 3.07 to 2.95 eV with increase in annealing temperature as inferred from photoluminescence and diffuse reflectance studies.

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► High aspect ratio anatase-titania nanotube powders were synthesized electrochemically.
► The surface area of the nanotubes were much higher than those reported.
► The annealing temperature limit for maintaining tubular morphology was established.
► The photoluminiscence spectroscopy reflected the presence of defects, annealing of defects and phase transformation.
► The nanotubes were of ∼5 nm wall thickness as revealed by TEM studies.