TiO2
sol was prepared hydrothermally in an autoclave from aqueous
TiOCl2
solutions as a starting precursor. Titanate nanotubes were obtained when the sol–gel-derived
TiO2
sol was treated chemically with a 10 M NaOH solution and subsequently heated in the autoclave at
150 °C
for 48 h. The samples were characterized using XRD, TEM, SEM, EDX, Raman
spectroscopy, and a BET surface area analyser. The effect of post treatments, such
as washing with and without hydrochloric acid and calcination, on the phase
structure, shape and morphology, pore structures, and BET surface area of the
titanate nanotubes was investigated. When a sample containing 7.08 wt% Na (after
washing only with water) was calcined at different temperatures from 300 to
900 °C, it showed the formation of a mixture of sodium trititanates and sodium hexatitanates
and was found to preserve the tubular morphology at higher temperatures.
However, a sample containing 0.06 wt% Na obtained after prolonged washing
with hydrochloric acid followed by heat treatment showed the formation of
TiO2 anatase
involving TiO2
(B) as an intermediate at lower temperatures and anatase was further transformed to the rutile
phase when the temperature was raised. On the basis of different observations, a general formula
NaxH2−xTi3O7·nH2O
has been proposed for the trititanate nanotubes.
Transition metal doped TiO2 (Ni, Fe, Cu) and nanocomposite TiO2 powders with rutile
phase were synthesized by mechanical alloying and heat treatment, and were characterized by
XRD, TEM, UV-DRS, and PL (Photoluminescence). Photocatalytic activity was also investigated
with the degradation rate of 4-chlorophenol and measured by total organic carbon analyzer. TEMEDP
and XRD patterns showed that the transition metal doped powders (only alloyed powder) were
in the form of rutile phase with the particle size of 20-30 nm. The average grain size of transition
metal doped powders was in the range of less than 10 nm. However, after heat treatment, the
alloyed powder formed composite of the titanate and rutile phase. The UV-DRS and PL
investigation showed that Ni doped 8 wt% nanocomposite TiO2 had the higher wavelength range
(600-660 nm) (2.0-1.9 eV) than that of the commercial P-25 powder(380-400 nm) by Degussa Co.
indicating that the Ni 8 wt% doped nanocomposite TiO2 shifted the absorption into the visible light
region and thus, enhanced the photocatalytic activity. Further, these results agreed well with TOC
investigation. Formation of titanate in transition metal doped TiO2 due to heat treatment was found
to control the grain growth of nano-sized TiO2 and to enhance its thermal stability at high
temperature.
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