Combination of self-propagating high-temperature synthesis (SHS) from Ti + B powder mixture followed by spark plasma sintering (SPS) is introduced for the fabrication of titanium diboride. Oxide impurities, including zirconium oxide and titanium oxide, are identified in the synthesized powders: the first one coming from the milling process after SHS to minimize agglomeration and the second one is a common oxide fine layer on particle surface. Both oxide phases are reduced during SPS treatment. Results confirm that increasing the SPS temperature enhances the reduction of ZrO₂, facilitating the incorporation of Zr cations into the lattice through substitution at Ti sites, thus allowing the formation of this solid solution diboride: Ti 1-xZr xB 2. The key finding is that the presence of a small amount of Zr cation, with higher atomic radius in TiB 2 crystal structure results in crystal distortion and it creates significant solid solution hardening effect as well as an improved wear response.