Abstract. Magnesium carbonate (MgCO 3 ) hollow nanospheres and their structural and thermal properties are presented. The hollow nanospheres are prepared via a microemulsion-based synthesis using dibutylmagnesium(II) and CO 2 as the starting materials. Size, structure, and composition of the as-prepared MgCO 3 hollow nanospheres are comprehensively validated by different analytical methods (SEM, STEM, TEM, XRD, FT-IR, TG). Accordingly, they exhibit an outer diameter of 35 Ϯ 9 nm, an inner cavity size of 17 Ϯ 5 nm, and a wall