ZrB2 and B4C are one of the most significant advanced ceramics. They are being used in various industrial areas from space technology to nuclear industry owing to their physical properties such as high melting point, high thermal/electrical conductivity and low density. Present study was conducted in two main stages: Self-propagating high-temperature synthesis (SHS) reactions and leaching. ZiO), Carbon black, B2O3 were used as starting material to produce ZrB2-B4C powders by SHS. Also Mg powder was used as the reductant. The reaction mixtures (approximately 100 g) were mixed thoroughly 15 minutes in a turbula mixer and charged into Cu crucible and compacted. W (tungsten) wire was placed at the top of copper crucible and the reaction realized by passing current through the wire. After initiation, a highly exothermic reaction became in a self-sustaining mode and propagated throughout the SHS mixture. The samples were characterized by using AAS and X-Ray Diffraction.