This study reports a room temperature mechanochemical route for the synthesis of LaB 6 powders originated from related metal oxide powders as La 2 O 3 and B 2 O 3 . Ca granules and B 2 O 3 powders were respectively used as reducing agent and boron source in the experiments. This study is actually meaningful to create added value by using the native boron source of Turkey for the production of high-technology boron materials. Milling duration as the most important parameter of mechanochemistry was examined to reveal the ideal production conditions. Mechanochemically synthesized powders were subjected to selective HCl leaching in order to eliminate unwanted phases. Thermochemical software of HSC Chemistry TM program was utilized to determine the reaction probability and to estimate the predicted products. Characterization investigations were carried out by X-ray diffractometer (XRD), differential scanning calorimeter (DSC), particle size analyzer (PSA), stereomicroscope (SM), scanning electron microscope (SEM), transmission electron microscope/energy dispersive spectrometer (TEM/EDS) and atomic absorption spectrometer (AAS). Nanosized LaB 6 powders were achieved with/without an insignificant amount of Ca 3 (BO 3 ) 2 phase via mechanochemistry in a high-energy ball mill for 3 h and via leaching with 4 M and 6 M HCl. Lastly, the experimental outputs obtained by a calciothermic reduction were compared with those of magnesiothermic reduction.