Phosphonate-containing mesoporous silica (PMPS) spheres were successfully synthesized using diethyl (2-bromoethyl)phosphonate and non-ionic and cationic surfactants. The spherical PMPS particles with the mesopores were effectively formed under the basic condition through the hydrolysis and condensation reactions of tetraethoxysilane, even though the BET surface area of the particles decreased with increasing the added phosphonate amount. The hollow structures with the mesopores were obtained in the preferential amount of the phosphonate. (C) 2019 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.