In this study, synthesis and characterization of elemental boron which is one of the high valuable boron-end products were carried out by mechanochemical method starting from anhydrous boron oxide. Metalic magnesium powder was used in the reducing process. Boron oxide and magnesium which has different grinding times and different ratios of reactant was ground at inert atmosphere and room temperature. The milled powder was applied to the heat treatment in an oven. Characterization of the synthesized powder was carried out by X-Ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrometry (EDS) and titration method. According to the XRD analysis, elemental boron phase was observed in an obtained product as a result of 1/3.3 powder to ball weight ratio milled 600 minutes. After the leaching purification process the results of XRD, EDS and titration analysis have shown that impurities was removed at significant rate. Purity of elemental boron has been determined as 95% by titration method.