Rapid breakdown anodization technique for the synthesis of high aspect ratio and high surface area anatase TiO{sub 2} nanotube powders

Journal Article · Tue Mar 15 00:00:00 EDT 2011 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2011.01.020· OSTI ID:21494235

Antony, Rajini P ^[1]; Mathews, Tom ^[1]; Dasgupta, Arup ^[2]; Dash, S; Tyagi, A K ^[1]; Raj, Baldev ^[1]

---

1. Thin Films and Coatings Section, Surface and Nanoscience Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamil Nadu (India)
2. Physical Metallurgy Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102, Tamil Nadu (India)

Clusters of high aspect ratio, high surface area anatase-TiO{sub 2} nanotubes with a typical nanotube outer diameter of about 18 nm, wall thickness of approximately 5 nm and length of 5-10 {mu}m 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 ({approx}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. -- Graphical abstract: Display Omitted Research highlights: {yields} High aspect ratio anatase-titania nanotube powders were synthesized electrochemically. {yields} The surface area of the nanotubes were much higher than those reported. {yields} The annealing temperature limit for maintaining tubular morphology was established. {yields} The photoluminiscence spectroscopy reflected the presence of defects, annealing of defects and phase transformation. {yields} The nanotubes were of {approx}5 nm wall thickness as revealed by TEM studies.

• OSTI ID: 21494235
• Journal Information: Journal of Solid State Chemistry, Vol. 184, Issue 3; Other Information: DOI: 10.1016/j.jssc.2011.01.020; PII: S0022-4596(11)00021-1; Copyright (c) 2011 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
ANNEALING
ANODIZATION
ASPECT RATIO
ELECTROCHEMISTRY
EV RANGE 01-10
MORPHOLOGY
NANOTUBES
PHASE TRANSFORMATIONS
PHOTOLUMINESCENCE
RUTILE
SCANNING ELECTRON MICROSCOPY
SPECTROSCOPY
SURFACE AREA
SYNTHESIS
TEMPERATURE RANGE 0273-0400 K
TEMPERATURE RANGE 1000-4000 K
TITANIUM OXIDES
TRANSMISSION ELECTRON MICROSCOPY
X-RAY DIFFRACTION
CHALCOGENIDES
CHEMICAL COATING
CHEMISTRY
COHERENT SCATTERING
CORROSION PROTECTION
DEPOSITION
DIFFRACTION
DIMENSIONLESS NUMBERS
ELECTROCHEMICAL COATING
ELECTROLYSIS
ELECTRON MICROSCOPY
EMISSION
ENERGY RANGE
EV RANGE
HEAT TREATMENTS
LUMINESCENCE
LYSIS
MATERIALS
MICROSCOPY
MINERALS
NANOSTRUCTURES
OXIDE MINERALS
OXIDES
OXYGEN COMPOUNDS
PHOTON EMISSION
RADIOACTIVE MATERIALS
RADIOACTIVE MINERALS
SCATTERING
SURFACE COATING
SURFACE PROPERTIES
TEMPERATURE RANGE
TITANIUM COMPOUNDS
TRANSITION ELEMENT COMPOUNDS