Y2O3/TiO2 composite hollow spheres were obtained by coating the as prepared PSA/yttrium compounds particles with an amorphous titanium layer and subsequent calcining at elevated temperatures in air. The size Of Y2O3/TiO2 composite hollow spheres was about 550nm. SEM, TEM, TG-DTG, IR and XRD characterized the samples by studied, respectively. The results showed that Y2O3/TiO2 composite hollow spheres were obtained when the ratio of yttrium compounds coating content and titanium compounds coating content was lower, whereas Y2Ti2O7 particles were formed and the Y2O3/TiO2 composite hollow spheres were crashed when the ratio of yttrium compounds coating content and titanium compounds coating content was higher.