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A C/SiO₂ composite was produced from 3-aminophenol and tetraethyl orthosilicate (TEOS) by a synthesis protocol that involved microwave irradiation. This protocol featured simultaneous 3-aminophenol polymerization and TEOS hydrolysis and condensation, which were achieved rapidly in a microwave reactor. The SiO₂ component was formed from low-concentration TEOS confined in cetyltrimethylammonium bromide micelles. We demonstrated a control of the SiO₂ particle size, ranging from 20 to 90 nm, by varying the 3-aminophenol concentration. The carbon component provided a microporous structure that greatly contributed to the high specific surface area, 375 m²/g, and served as a host for the nitrogen functional groups with a content of 5.34%, 74% of which were pyridinic type. The composite formation mechanism was clarified from time-series scanning electron microscopy images and dynamic light …