In order to obtain a multifunctional nanocomposite material-for electrochemical sensors and photocatalytic applications, structures based on Bi, Fe and TiO2 were grown inside carbon xerogel supports (BiFeCX and BiFeCX-TiO2). First, a wet polymer containing Bi and
Fe salts was obtained by following a modified resorcinol-formaldehyde based sol–gel route, followed by drying in ambient conditions, and pyrolysis under inert atmosphere. Then, through TiCl4 hydrolysis, TiO2 nanoparticles were deposited on the BiFeCX xerogel leading
to BiFeCX-TiO2. The morphological and structural characterization of the investigated nanocomposites consisted in X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and N2 adsorption measurements, revealing
porous carbon structures with embedded nanoparticles and the particularities driven by the pyrolysis and TiCl4 treatment. The new modified electrodes based on BiFeCX or BiFeCX-TiO2 nanocomposite materials, kept in a chitosan matrix (Chi) and deposited on a glassy carbon
(GC) electrode surface (GC/Chi-BiFeCX or GC/Chi-BiFeCX-TiO2), were obtained and investigated for Pb(II) voltammetric detection and H2O2 amperometric detection. Moreover, the BiFeCX-TiO2 nanocomposite was tested for the photocatalytic degradation
of methyl orange. The great potential of BiFeCX nanocomposite material for developing electrochemical sensors, or BiFeCX-TiO2 for sensors application and photocatalytic application was demonstrated.