Zirconium diboride (ZrB 2 ) ceramic nanoparticles were synthesized by using zirconium (IV) complexes as new precursors. The citrate sol-gel process, which included the mixing of ions at the atomic scale, affected hydrolysis reactions and finally led to the formation of the pure phase of the sample. Results showed that the different sizes of ZrB 2 nanocrystals were produced by adjusting four potential chelating agents of bi-and tetradentate (N 2 O 2 donor set) ligands by the sol-gel process during carbothermal reduction.The samples were characterized by TGA, XRD, FTIR, FESEM, and TEM. The results were obtained from microscopic observations indicated that pure and homogeneous ZrB 2 nanostructures have been formed by using 2-hydroxyacetophenone (hap).