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Activators generated by electron transfer (AGET) for atom transfer radical copolymerization (ATRP) was employed to synthesize tailor‐made random poly (styrene‐co‐methyl methacrylate)/mesoporous kieselgur nanocomposites. Some inherent features of the mesoporous kieselgur platelets were studied by nitrogen adsorption/desorption isotherm and transmission electron microscopy images. Conversion and molecular weight determinations were carried out using gas chromatography and size exclusion chromatography respectively. Addition of 3 wt.% mesoporous kieselgur platelets results in increments of conversion from 72 % to 87 % and molecular weight of copolymer chains from 15986 g mol−1 to 18564 g mol−1 respectively; however, polydispersity index values increases from 1.19 to 1.48. Increasing thermal stability of the nanocomposites is demonstrated by thermogravimetric analysis. Differential scanning calorimetry shows an increase in glass transition temperature from 70.6 °C to 75.7 °C by adding 3 wt.% of mesoporous kieselgur platelets. [ABSTRACT FROM AUTHOR]