Small titania particles were generated within the template of a non-ionic s
urfactant (TX-100) reverse micelle assembly by the sol-gel method from tita
nium(IV) isopropoxide. Cyclohexane was used as the reaction solvent to form
a reverse micelle system with a low water to surfactant ratio. Gelling, i.
e., hydrolysis and polycondensation, were observed by means of viscosity me
asurements. The transparent raw gels obtained were dried under vacuum at 37
2 K. The dry gels were then either thermally decomposed directly to TiO2 or
the organic content (surfactant) was substantially reduced first by superc
ritical fluid extraction with CO2 and then thermally treated. Special atten
tion was paid to the effect of temperature on the extent of crystallisation
of individual crystallographic phases of TiO2. Gels, partly decomposed gel
s and gels after the supercritical fluid extraction were investigated by XR
D, XPS, IR, TPR, thermogravimetry, mass spectrometry, elemental analysis, U
V-vis, SEM and extensive gas adsorption measurements. Their properties were
related to the structure and other features of the final nanosized TiO2 pa
rticles. The anatase form of TiO2 with a very high specific surface area an
d well-developed mesoporous and microporous structure was prepared.