Rifampicin nanoparticles (RF NPs) was sunthesized by lyophilization method and characterized by using scanning electron spectroscopy (SEM) and atomic force spectroscopy (AFM). It is found that the dimension of the RF NPs was 85.74 nm. An electrochemical measurement approach has been used to examine the effects of various temperature degrees for a range of 30-70 °C on the redox current peaks of RF NPs in the KCl solution as an electrolyte. The results of the electrochemical analysis of RF NPs in KCl solution were obtained by the cyclic voltammetric method to find two oxidation peaks (I,II) at +900 and +225 mV, also two reduction peaks appeared at -680 and -300 mV. They were studied at different temperatures to identify the values of the activation energies (E a * ) of these peaks by Arrhenius equation as well as their thermodynamic values using the Eyring equation to determine the values of Gibbs activation energy (ΔG*), activation enthalpy (ΔH*), and activation entropy (ΔS*). RF NPs were analyzed through the effect of different temperatures on both the oxidation and reduction peaks, which showed that the high temperature leads to a catalytic state as an electrochemicalcatalyst.