Cobalt boride (Co 2 B) is a significant transition metal boride having a wide range of usage area due to its high oxidation, abrasion and corrosion resistance as well as its superior electrochemical, magnetic and anisotropic properties. In this study, pure Co 2 B nanocrystals were synthesized with Co, B 2 O 3 and Mg as starting materials via the mechanochemical synthesis (MCS) method by high-energy planetary ball mill in a hardened steel vial with hardened steel balls. All the experiments were conducted under Ar atmosphere at different rotational speeds and at 20 : 1-30 : 1-40 : 1 ball-to-powder ratios. Leaching of Co 2 B + MgO powder mixtures occurred after milling and purified with acetic acid and pure Co 2 B nanocrystals were obtained in solid form. The Co 2 Bs were characterized through X-ray diffraction, scanning electron microscopy, vibrating sample magnetometer, Brunauer-Emmett-Teller and specific density analyses, and effects of synthesis parameters on product properties were revealed. Surface areas of the powders synthesized at 40 : 1 ball-to-powder ratio at different rotational speeds were measured as 21.14, 40.36 and 52.33 m 2 g −1 , respectively. Crystallite sizes of Co 2 B nanocrystals were between 7.27 and 9.84 nm and their specific density varied between 7.61 and 7.78 g cm −3. It was determined that all samples were saturated and exhibited hysteresis and ferromagnetic behaviours, and saturation magnetization was between 35 and 50 emu g −1 .