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.
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