Abstract: The core-shell polystyrene/silica composite microspheres with tailored dimensions and compositions were prepared by layer-by-layer self-assembling. The polymer cores were removed by calcination
and hollow silica spheres with tailored wall thickness were produced. TEM photographs showed that silica nanoparticles formed a uniform shell round the core, which turned into a clear-cut
hollow sphere after calcination. TG revealed that silica content within the composite microspheres increased with the assembled nano silica diameter. Both the successful assembly of
SiO₂ and the complete removal of PS can be verified by FIIR comparison of PS, SiO₂, composite microspheres and the powders after heating treatment. With the same number layers
of nanoparticles adsorpted on the latex cores, the larger the selected SiO₂ nanoparticles diameter (10nm, 20nm, 40nm), the larger the composite microspheres diameter, and the thicker the hollow spheres’ wall.

Key words: self-assembly, PS/SiO₂ composite microspheres, hollow silica spheres