Boron Neutron Capture Therapy (BNCT) is a promising therapy for the cure of diffuse tumors. The successful clinical application of BNCT requires finding new boron-based compounds suitable for an efficient 10B delivery to the cancerous tissues. The purpose of this work is to synthesize borosilicate nanoparticles by a sol–gel recipe, and to functionalize them with folic acid in order to promote their capture by the tumor cells. Whereas sol–gel is a promising technique for the synthesis of nanoparticles, in case of borosilicate systems this approach is affected by significant boron loss during preparation. Here we show that functionalization of borosilicate nanoparticles with folic acid can reduce the boron loss. Moreover, preliminary biocompatibility tests indicate that functionalization strongly changes the reactivity of NPs towards blood cells, so favouring the potential use of these materials for clinical applications.