Abstract: LaB6 micropowder was prepared by self-propagating high-temperature synthesis (SHS). SHS process in which the thermally explosible and leachable products were checked by XRD, then a two-step leaching procedure was therefore confirmed. The LaB6 prepared was analyzed and characterized by TEM, spectral analysis, SEM and granularity analyzer. The results indicate that the thermally explosible products consist of LaB6, MgO and bits of Mg3B2O6 and LaOCl, and that the single pure phase LaB6 can be obtained using HC1 then H2SO4 in an interlacing way in leaching process. The crystal lattice constant of LaB6 was calculated as a = 0.4148 nm, with its purity lower than 99% and the mean grain size is 1.92 μm.