CeO 2 -ZrO 2 composite nanoparticles with mesoporous and spherical morphologies were assembled into different homogeneously dispersed, domain, and core-shell structures by changing the reaction conditions, such as the heating rate, acid, and solvent, in supercritical alcohols. Ce x Zr 1-x O 2 with homogeneous structures were prepared from Ce(NO 3 ) 3 and ZrO(NO 3 ) 2 in the presence of formic acid in methanol by rapid heating (500 °C/min) to 300 °C, while CeO 2 -ZrO 2 with domain structures were obtained by slow heating (5.4 °C/min). Treatment of mesoporous and spherical ZrO 2 nanoparticles with a Ce(NO 3 ) 3 solution in supercritical conditions yielded CeO 2 -ZrO 2 nanocomposites with core-shell morphologies, while solvents playing a key role in controlling the thickness of the outer shell; methanol produced a very thin outer shell structure of cubic CeO 2 and 2-propanol afforded a thick one.