Core-shell tunable monodispersed carbon nanospheres

A novel strategy for the synthesis of core–shell carbon nanospheres (CNS) with tunable architectures is presented, utilizing hydrothermal carbonization (HTC) of glucose. By modulating feed-injection dynamics, reaction time, and concentrations of key intermediates—formic acid (FA) and levulinic acid (LA)—precise control over CNS morphology and structural properties was achieved. FA was found to enhance shell formation by accelerating dehydration and surface polymerization reactions, while LA facilitated core growth via aldol condensation and structure-directing crosslinking agent during early nucleation stages. The interplay of these intermediates enabled fine-tuning of the core-to-shell ratio, with advanced characterization ( 13 C MAS NMR, FTIR, XPS, XRD, and Raman) confirming the transition from hydroxymethylfurfural-driven nucleation to aromatic-rich structures. This study provides a comprehensive understanding of HTC mechanisms and establishes a versatile platform for designing hierarchical carbon materials for diverse applications.