Nanoparticles composed of inorganic boron-containing compounds represent a promising candidate as ¹⁰B carriers for BNCT. This study focuses on the synthesis, characterization, and assessment of the biological activity of composite nanomaterials based on boron carbide (B₄C). Boron carbide is a compelling alternative to borated molecules due to its high volumetric B content, prolonged retention in biological systems, and low toxicity. These attributes lead to a substantial accumulation of B in tissues, eliminating the need for isotopically enriched compounds. In our approach, B₄C nanoparticles were included in composite nanostructures with ultrasmall superparamagnetic nanoparticles (SPIONs), coated with poly (acrylic acid), and further functionalized with the fluorophore DiI. The successful internalization of these nanoparticles in HeLa cells was confirmed, and a significant uptake of ¹⁰B was observed. Micro-distribution studies were conducted using intracellular neutron autoradiography, providing valuable insights into the spatial distribution of the nanoparticles within cells. These findings strongly indicate that the developed nanomaterials hold significant promise as effective carriers for ¹⁰B in BNCT, showcasing their potential for advancing cancer treatment methodologies.