A nanocomposite with an FeOOH/SiO2ratio equal to 17.7 wt% and the pertinent matrix, obtained by etching away the nanoparticles through reaction with hydrochloric acid, were investigated by XRD, TGA-DTA, heliostereopicnometry, BET, and TEM techniques. The study shows the presence in the nanocomposite of ferrihydrite nanoparticles phase with average dimensions around 4 nm. The FeOOH nanoparticles structure was analyzed by synchrotron X-ray diffraction data using the distribution difference curve method. The porous structure of the matrix resulting by etching away the nanoparticles differs significantly from that of a pureSiO2sample obtained by hydrolysis of TEOS under the same operative conditions followed in the nanocomposite preparation.