Structural, Morphological, and Textural Characterization of Ni- and Fe-Based KCC-1@C Hybrid Nanocomposites

Hybrid nanocomposites composed of dendritic fibrous nanosilica (DFNS) identified as KCC-1 and resorcinol–formaldehyde (RF) resin were synthesized via the polymer-assisted deposition (PAD) method for the incorporation of Ni and Fe in mono- and bimetallic configurations. The RF resin enabled uniform dispersion Fe-based and Ni-based nanoparticles through coordination with functional groups, while KCC-1 provided a high-surface-area, mesoporous support. A comprehensive structural and chemical characterization confirmed the formation of hematite in the Fe-based system; NiO and metallic Ni in the Ni-based material; and FeO, NiO and metallic Ni in the bimetallic composite, in the form of well-dispersed metal nanoparticles between 3–6 nm. Although a reduction in BET surface area was observed due to resin and metal loading, all nanocomposites retained mesoporous structures with Type IV isotherms and H3-type hysteresis, suitable for catalytic applications. The nanocomposites exhibited structural stability up to 800 °C under N2, with a total mass loss of 12–14% dominated by moisture desorption below 100 °C (~8–11%) and minor surface group degradation at higher temperatures. These findings demonstrate the potential of the PAD method for fabricating functional hybrid materials with improved metal dispersion.