This study reports on the preparation of diiron boride (Fe2B) powders via mechanochemical synthesis (MCS) followed by a purification step and on the embedment of pure Fe2B nanoparticles into silica (SiO2) nanospheres. Fe2O3, B2O3 and Mg powders used as starting materials were blended in stoichiometric amounts and mechanochemically synthesized up to 7 h in a high-energy ball mill. As-synthesized powders were purified from the undesired Mg-based by-products by HCl leaching. After that, pure Fe2B nanoparticles with sizes of smaller than 40 nm were embedded in SiO2 nanospheres using a tetraethyl orthosilicate (TEOS) and ammonia (NH3) containing solution. Characterization investigations of the as-synthesized, leached and SiO2-embedded powders were carried out using X-ray diffractometer (XRD), scanning electron microscope/energy dispersive spectrometer (SEM/EDS), particle size analyzer (PSA), transmission electron microscope (TEM), Fourier transform infrared spectrometer (FTIR) and vibrating sample magnetometer (VSM). The average particle size of the Fe2B incorporated SiO2 nanospheres was measured as about 330 nm. Magnetic measurements revealed that pure Fe2B powders and their SiO2-embedded samples had soft ferromagnetic behaviour with coercivity of 125 and 168 Oe, respectively.