Y. Tanaka et al., PREPARATION OF TRANSLUCENT AND POLYCRYSTA LLINE TIO2 MONOLITH FROM METAL ALKOXIDE SOLUTION, Nippon Seramikkusu Kyokai gakujutsu ronbunshi, 102(6), 1994, pp. 578-582
Translucent and polycrystalline TiO2 monolith was prepared by heating
a gel at 500-degrees-C. Clear TiO2 gel as a precursor was formed throu
gh the controlled hydrolysis of a Ti-n-butoxide/cyclohexane solution i
n a vessel covered with a plastic film having pin-holes. Upon heating,
the amorphous gel crystallized to anatase at 200-degrees-C and conver
ted into rutile at 600-degrees-C. In the temperature range from room t
emperature to 600-degrees-C, a large volume change which may cause a c
rack in the gel occurred with decomposition of residual organic materi
als. Transparency of the gel was retained up to 550-degrees-C except i
n the decomposition temperature range of organic materials (160-330-de
grees-C). The TiO2 monolith obtained from a crak-free gel after heatin
g to 500-degrees-C at a rate of 20-degrees-C/h was a translucent porou
s material (apparent porosity: 42% and pore diameter : 7-30 nm) and co
nsisted of fine anatase grains.