Synthesis and properties of nanoparticulate titanium dioxide compounds

Abstract

An electrolytic cell was designed and constructed for the preparation of TiO2 nanotubes. Conditions of anodic oxidation were established to reproducibly prepare TiO2 nanotubes of average length 35-50 μm vertically orientated relative to the plain of a pure titanium metal sheet. A non-aqueous solution of ethylene glycol containing small percentage of ammonium fluoride was used as the electrolyte with an applied voltage of 60 V. The morphology and dimensions of the nanotube arrays were studied by scanning (SEM) and transmission (TEM) electron microscopy. The effect of calcination under different conditions of temperature and atmosphere (nitrogen, argon and air) were assessed by both X-ray diffraction (XRD) and cyclic voltammetry (CV). Cyclic voltammetry studies were made possible by construction of a specially designed titanium electrode upon which the nanotubes were prepared. CV studies established a positive correlation between crystallinity and conductivity of the nanotubes. Doping of the nanotubes with nitrogen and carbon was established by elemental analysis, X-ray photoelectron spectroscopy (XPS) and Rutherford back scattering (RBS). The effect of nonmetal doping on the band gap of the TiO2 nanotubes was investigated by diffuse reflectance spectroscopy (DRS).