Medium sized spherical particles of Li2TiO3 (with diameters below 100 mi m) can be prepared from peroxy lithium titanate solution (stabilized with citric acid) by a modified INCT variant of the sol-gel process. The process consists of the following main steps: (I) formation of aqueous phase emulsion in 2-ethylhexanol-1 containing the surfactants 1v/o SPAN-80 and 1v/o Ethomen S-15 (EH); (II) gelation of emulsion drops by extraction of water with partially dehydrated EH; (III) filtration and washing with carbon tetrachloride or acetone; (IV) non-destructive thermal treatment. The tritium release from sol-gel process preparation of Li2TiO3 micro-spheres was found very close to that observed for other traditional material however, the new process is more efficient than other processes because of the morphology of the sintered specimens