In this study, Bi-Ce Oxide nanostructures were prepared via a new and facile method. To find the optimal conditions for the synthesis of Bi-Ce Oxide nanostructures, the effect of some synthesis parameters was examined. The results of this work showed that the size and morphology of Bi-Ce Oxide nanostructures were significantly affected by the examined parameters. The as-synthesized Bi-Ce Oxide nanostructures were characterized by FT-IR, FESEM, EDS and XRD. The obtained outcomes displayed that with the aid of this new procedure can be made sphere-like Bi-Ce Oxide nanostructures with good uniformity. Also, the photocatalyst activity of as-prepared Bi-Ce oxide nanostructures was examined by removal of the organic pollution under visible light.