In this study, producabilityof Al2O3/B4C ceramic phases at room temperaturecontrary high temperatureproduction methods (carbothermal reduction, sol gel, chemical vapor deposition etc.) using the ternary system of B2O3-Al-C was investigated as mechanochemical. The starting materials were activated in attritor, planetary and spex ball mill under argon atmosphere at different times. The characterization of ceramic phase powder mixtures synthesized was investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) XRD studies showed that Al2O3/B4C ceramic phases were formed by using spex after 10h of milling. The agglomeration phenomenon with decrease (50-200 nm) in the powder size were determined as a result of mechanical energy and increase in amount ofceramic phaseformed. TEM studies showed that the products after the leaching process were yielded the efficient distributionofthe ceramic phases with the removal of contaminations.