In this study, nanoparticle boron carbide was produced after the reduction of boron oxide with magnesium under the presence of carbon by using mechanochemical synthesis method. During the synthesis processing, microstructure and phase transformations of powders were performed by using X-ray diffraction (XRD), Fourier-transform infrared spectrum (FT-IR), scanning electron microscope (SEM), and high-resolution transmission electron microscopy (HRTEM). At the end of 2 h, reaction products (MgO, B4C) were determined by XRD and FT-IR examinations. Nanoparticle B4C single-phase crystalline structure from the MgO/B4C composite powder mixture, which was the reaction product, was obtained by leaching process. With the increase in the synthesis period, starting material peaks diminished and Fe peak intensity became evident. After the HRTEM examinations, it was determined that synthesized B4C particles were within range of 10–200 nm especially in the activation of leaching process. Additionally, by using spot pattern analysis method, planes represented by B4C particles were calculated.
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