In this thesis we made and evaluated different porous cathode electrodes based on the carbon nanoparticles prepared with ultrasonic method. Performance of these electrodes in electroreduction of thionyl chloride compare together in the cell and three-electrode system. The electrochemical behavior of four types of carbon acetylene black (AB), Vulcan XC-72, multi walled carbon nano tubes (MWCNTs) and carbon that refined from commercial battery was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperommetry (CA) techniques in 1.8 M LiAlCl 4 /SOCl 2 electrolyte. The CV data as depicted clearly show that the acetylene black carbon with 7mA cathodic current is the best carbon sample for the electroreduction of thionyl chloride. In addition, the results of polarization curves show that the acetylene black carbon has a maximum power density of 175 mW, which is higher than other carbons at 25?C, while MWCNTs with 160 mW maximum power density shows the lower activity among four types of the candidate carbons. Moreover, the effect of adding 2 mg poly(vinylpyrrolidone) (PVP) to the electrolyte was evaluated in three-electrode system by CV, LSV and CA techniques. The results of the electrochemical tests show that Vulcan XC-72 with 250 m 2 /g surface area is the best cathode in the presence of PVP, because the peak current of CV diagram of this carbon is three times higher than other carbons. The nanocomposite of Vulcan-PVP and MWCNTs-PVP was evaluated and compared in three-electrode system. The result of CV diagram show that Vulcan carbon nanocomposite with 6 mg PVP has the best performance for the Li/SOCl 2 battery.