A one‐step in‐situ route to free standing core–shell silicon carbide in graphene nanoparticles on monolayer graphene is presented. The core–shell SiC@Graphene nanoparticle growth is realized by a simple chemical vapor deposition (CVD) process where carbon and silica precursors are simultaneously introduced into the growth chamber. This process permits the synthesis of a monolayer graphene sheet dressed with silicon carbide nanoparticles in a single CVD step, with the product controlled by growth temperature and the carbon/SiO2 exposure time. Growth of a high density SiC@Graphene distribution on a continuous graphene layer requires long exposure times (>1 h) and high temperature (1000 °C). The growth process proceeds by a carbothermal mechanism. The simultaneous growth of graphene and SiC nanoparticles enables uniform core–shell SiC@Graphene nanoparticle formation rather than SiC/carbon nanofiber growth. As a proof of concept, the functionalization of preformed nanoparticle graphene surface with a diazonium salt is studied, demonstrating an increase in grafting rate with increasing nanoparticle population. This work provides a general procedure for one‐step synthesis, with further investigation required to develop precursors for hybrid core–shell CVD material growth.
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