The cyclic Voltammetry of zirconyl chloride with different concentrations was measured experimentally using DY2000 cyclic Voltammetry apparatus in 0.1M KF (potassium fluoride) as a supporting electrolyte. The silver electrode was used as a supporting working electrode. The other two electrodes in the three-electrode system are platinum wire and Ag / AgCl electrode immersed in saturated KCl solution. The redox mechanism was supported by reduction and/or oxidation. Effect of scan rate was also examined and the redox system is diffusion controlled.The different used scans are 0.1,0.02 and 0.01 Volt per Sec. The relation between iP and log scan rate was done to ensure the redox mechanism.It was concluded that zirconyl ions are hydrolyzed in 0.1M KF solutions forming hydroxyl complexes.