  To investigate excess-hydrolysis of titanium alkoxides, TiO2 powders were
fabricated from titanium-tetra-isopropoxide using 6:1 and 100:1 H2O:Ti (r)
ratios. Powders were dried and fired at a range of temperatures ( up to 800 C).
Hydroxylation and organic content in powders were characterised using ATR-FTIR,
laser Raman microspectroscopy, and elemental microanalysis; surface area and
pore size distribution were evaluated using N2 gas adsorption; phase
composition was analysed using XRD and laser Raman microspectroscopy; and
crystallite size was evaluated by XRD, TEM and SEM. Results showed
near-complete hydrolysis in a predominantly aqueous medium (r = 100), resulting
in precipitated crystalline powders exhibiting brookite and anatase, which
begin to transform to rutile below 500 C. Powders precipitated in a
predominantly organic medium (r = 6) underwent partial hydrolysis, were highly
porous and exhibited an amorphous structure, with crystallisation of anatase
occurring at 300 C and transformation to rutile beginning at 500 to 600C.
