The aim of this study is to highlight the use of polystyrene (PS) latexes stabilized with block copolymers as a hard template in the production of metal oxide hollow spheres. PS latexes produced by dispersion polymerization by stabilizing with tertiary amine methacrylate-based diblock copolymer were used as a hard template in the preparation of nickel manganese oxide (NiMn 2O 4) hollow spheres and cobalt iron oxide (CoFe 2O 4) bowl-like structures. Thanks to the diblock copolymer stabilizer with tertiary amine functional groups on the PS surface, precursor salts of CoFe 2O 4 and NiMn 2O 4 were first homogeneously deposited on the surface of PS latexes with a controlled precipitation technique. Then, metal oxide hollow spheres and bowl-like structures were produced by calcination. XRD results showed that CoFe 2O 4 and NiMn 2O 4 structures were successfully obtained after calcination. The thermogravimetric analysis results showed that the CoFe 2O 4 and NiMn 2O 4 contents of the hybrid PS spheres were in the range of 26.0–28.6 wt%. SEM images showed that the inorganic-polymer spheres fused with each other after calcination to form larger magnetic CoFe 2O 4 bowl-like structures. SEM images also indicated successful production of highly rough NiMn 2O 4 hollow spheres with nanosheets on the surface.
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